CN104372169A - Method of extracting tungsten from high-barium tungsten ore - Google Patents
Method of extracting tungsten from high-barium tungsten ore Download PDFInfo
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- CN104372169A CN104372169A CN201410734362.3A CN201410734362A CN104372169A CN 104372169 A CN104372169 A CN 104372169A CN 201410734362 A CN201410734362 A CN 201410734362A CN 104372169 A CN104372169 A CN 104372169A
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- tungsten
- ore
- roasting
- tungsten ore
- barium
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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 discloses a method of extracting tungsten from high-barium tungsten ore. The method includes: mixing the high-barium tungsten ore and a certain amount of SiO2 and Na2CO3 to obtain mixture, roasting the mixture at the high temperature, and leaching roasting slag with Na2CO3 to obtain tungsten. By roasting the Na2CO3 and SiO2, the structure of the high-barium tungsten ore is fully broken to obtain stable (Ba or Ca)2SiO4 slag which is leached with high-concentration Na2CO3, water-soluble calcium and barium ions in roasting material are deposited, deposition of tungsten ions is prevented, leaching rate of the tungsten is greatly increased, reaching greater than 95%, and the problem that the high-tension alkaline leaching methods of the prior art fail to break the barite structure, leading to low leaching rate, is solved. The method according to the technical scheme is simple to operate, raw materials are cheap, processing can be performed with traditional equipment, and the method fully satisfies industrial production.
Description
Technical field
The present invention relates to a kind of method extracting tungsten from high barium tungsten ore, belong to tungsten ore technical field of smelting.
Background technology
The main raw materials for metallurgy of tungsten is wolframite and sheelite, but along with the exploitation year by year of tungsten resource, it presents grade reduces, component mechanism is complicated and with other metal associations etc., the ore dressing of tungsten resource and smelting cost are raised.
The common method of present process wolframite and sheelite is high pressure base leaching, this technique is under high-alkali, high-temperature and high-pressure conditions, tungsten ore can be made to be decomposed, and make W content in slag be reduced to less than 1 ~ 3%, but condition needed for this technique and equipment harshness, and this technique can not destroy barite structure, be not suitable with containing high barium tungsten ore.
Same for sour decomposition method, due to BaSO
4be insoluble to acid, and part barite and white tungsten composition disperse to exist, even if therefore the heteropolyacid treatment process mentioned in patent is also inapplicable.
And the common treatment process containing high barium material, then adopt the method for pyrocarbon reduction, by BaSO
4reduction generates water-soluble BaS or BaCl
2(adding chlorizating agent when reducing), thus destroy barite structure, reach the extraction of object element.
Summary of the invention
For the defect that the technology extracting tungsten in prior art from high barium tungsten ore exists, the object of the invention is to be to provide one effectively can destroy high barium tungsten ore structure, the efficient method leaching tungsten ore, the method is simple to operate, and cost is low, meets demand of industrial production.
The invention provides a kind of method extracting tungsten from high barium tungsten ore, the method is after being pulverized by high barium tungsten ore, with silicate and/or SiO
2, and Na
2cO
3mixing, is after carrying out roasting under the condition of 800 ~ 1000 DEG C in temperature, and fired slags adopts concentration to be not less than the Na of 8g/L
2cO
3solution leaches, and obtains sodium tungstate solution; Wherein, silicate and/or SiO
2quality with SiO
2metering is 5 ~ 20% of high barium tungsten ore quality; Na
2cO
3molar weight be 2 ~ 4 times of tungsten molar weight in high barium tungsten ore.
The method extracting tungsten from high barium tungsten ore of the present invention also comprises following preferred version:
In preferred scheme, roasting time is 2 ~ 3h.
In preferred scheme, high barium tungsten ore is crushed to granularity within the scope of 74 ~ 200 μm.
Leaching in preferred scheme is carry out under temperature is the condition of 20 ~ 90 DEG C; Most preferably be and carry out under the condition of 50 ~ 90 DEG C.
In preferred scheme, extraction time is 0.5 ~ 3h; Most preferably be 0.5 ~ 1h.Extraction time is more than 1h, and tungsten leaching yield is almost constant.
In preferred scheme, fired slags adopts Na
2cO
3solution is crushed to granularity within the scope of 0.1mm ~ 1mm before leaching.Can produce a large amount of gas in roasting process of the present invention, fired slags is vesicular, therefore fired slags only need be crushed to 0.1mm ~ 1mm can reach good leaching effect.
In preferred scheme, sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Described high barium tungsten ore contains higher barite composition, and the dispersion of barite composition exists in tungsten ore or parcel tungsten ore.
Preferred scheme mesosilicic acid salt and/or SiO
2addition make suitable adjustment according to the number of actual silicon content in high barium tungsten ore.
The technological difficulties that the present invention solves: contriver makes a large amount of experimental studies to the technique that high barium tungsten ore extracts tungsten, research finds to add appropriate Na in high barium tungsten ore roasting process
2cO
3and SiO
2(or silicate), effectively can destroy the structure (original structure is that tungsten ore wraps up or is dispersed in tungsten ore by barite) of former high barium tungsten ore, Ba, Ca and Si in high barium tungsten ore are formed more stable (Ba, Ca)
2siO
4, adopt the sodium carbonate solution of high density to leach simultaneously, effectively can prevent CaSiO
3deng dissolving, and suppress tungsten precipitation further, substantially increase the leaching yield of tungsten.Technical scheme of the present invention efficiently solves high barium tungsten ore structure in prior art and is difficult to destroy, and causes the problem that tungsten leaching yield is low.
The beneficial effect that hinge structure the present invention brings: the high efficiency extraction 1, fully achieving tungsten in the low-grade high barium tungsten ore being difficult to utilize; 2, the auxiliary material additive adopted is cheap, and technique is simple, legacy equipment can be adopted to process, meet industrialization production requirements completely.
Accompanying drawing explanation
[Fig. 1] is the XRD figure of leached mud in embodiment 1, and wherein, B is Ba
1.55caO
0.45siO
4, W is BaWO
4, P is W
2o
3(PO
4)
2.
[Fig. 2] is the XRD figure of leached mud in embodiment 2.
[Fig. 3] is the XRD figure of leached mud in comparative example 1.
[Fig. 4] is the XRD figure of leached mud in comparative example 2.
Embodiment
Further illustrate below in conjunction with example, following instance is intended to further illustrate the present invention and is not the further restriction to invention.
Embodiment 1
Get a certain high barium tungsten ore 500g (its composition analysis is as table 1), be crushed to granularity 74 ~ 200 μm of scopes, with 270gNa
2cO
3and 40gSiO
2after mixing, put into corundum crucible, roasting 3h in the retort furnace of 850 DEG C.Calcining is through cooling, and being crushed to granularity is after 0.1mm ~ 1mm, with 10g/L NaCO
3solution, liquid-solid ratio controls at 5mL/g, 60 DEG C leach 1h.Gained sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Composition/the % of the high barium white tungsten concentrate of table 1
After leaching, analyze the W content in leach liquor and leached mud, leach liquor composition is wherein as table 2, and tungsten leaching yield is 95.96%, and leached mud XRD figure is as Fig. 1.Roasting process Ca, Ba, Si are formed comparatively stable (Ca, Ba)
2siO
4, leached mud XRD figure is as Fig. 1, and the formation of this material directly describes the method and can destroy BaSO
4structure, can reduce white tungsten in turnover process simultaneously and precipitate the high problem of the W loss that causes.
The composition analysis of table 2 leach liquor
Embodiment 2
Get a certain high barium tungsten ore 500g (its composition analysis is as table 1), be crushed to granularity 74 ~ 200 μm of scopes, with 270gNa
2cO
3and 70gSiO
2after mixing, put into corundum crucible, roasting 2h in the retort furnace of 950 DEG C.Calcining is through cooling, and being crushed to granularity is after 0.1mm ~ 1mm, with 20g/LNaCO
3solution, liquid-solid ratio controls at 4mL/g, 60 DEG C leach 1h.After leaching, analyze the W content in leach liquor and leached mud, the leaching yield obtained is 96.76%, and its leached mud XRD figure is as Fig. 2.Gained sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Comparative example 1
And when maturing temperature is lower than 800 DEG C, adopt the method Roasting And Leaching tungsten result as follows:
Get a certain high barium tungsten ore 50g (its composition analysis is as table 1), be crushed to granularity 74 ~ 200 μm of scopes, with 27gNa
2cO
3and 5gSiO
2after mixing, put into corundum crucible, roasting 3h in the retort furnace of 700 DEG C.Calcining is through cooling, and being crushed to granularity is after 0.1mm ~ 1mm, at NaCO
3in 10g/L solution, liquid-solid ratio controls at 5mL/g, leaches 1h at 60 DEG C.After leaching, analyze the W content in leach liquor and leached mud, the leaching yield obtained is 65.61%, and its leached mud XRD figure is as Fig. 3.Gained sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Comparative example 2
And roasting is not when adding silicon, gets a certain high barium tungsten ore 50g (its composition analysis is as table 1), be crushed to granularity 74 ~ 200 μm of scopes, with 27g Na
2cO
3after mixing, put into corundum crucible, roasting 3h in the retort furnace of 850 DEG C.Calcining is through cooling, and being crushed to granularity is after 0.1mm ~ 1mm, at NaCO
3in the solution of 10g/L, liquid-solid ratio controls at 5mL/g, leaches 1h at 60 DEG C.After leaching, analyze the W content in leach liquor and leached mud, the leaching yield obtained is 55.72%, and its leached mud XRD figure is as Fig. 4.Gained sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Comparative example 3
During leaching, directly go out with water logging, it is as follows that tungsten leaches result:
Get a certain high barium tungsten ore 50g (its composition analysis is as table 1), be crushed to granularity 74 ~ 200 μm of scopes, with 27gNa
2cO
3and 5gSiO
2after mixing, put into corundum crucible, roasting 3h in the retort furnace of 850 DEG C.Calcining is through cooling, and being crushed to granularity is after 0.1mm ~ 1mm, and liquid-solid ratio controls at 5mL/g, in 60 DEG C of water, leach 1h.After leaching, analyze the W content in leach liquor and leached mud, the leaching yield obtained is 89.56%.Gained sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
Claims (6)
1. from high barium tungsten ore, extract a method for tungsten, it is characterized in that, after high barium tungsten ore is pulverized, with silicate and/or SiO
2, and Na
2cO
3mixing, is after carrying out roasting under the condition of 800 ~ 1000 DEG C in temperature, and fired slags adopts concentration to be not less than the Na of 8g/L
2cO
3solution leaches, and obtains sodium tungstate solution; Wherein, silicate and/or SiO
2quality with SiO
2metering is 5 ~ 20% of high barium tungsten ore quality; Na
2cO
3molar weight be 2 ~ 4 times of tungsten molar weight in high barium tungsten ore.
2. method according to claim 1, is characterized in that, described roasting time is 2 ~ 3h.
3. method according to claim 1, is characterized in that, described high barium tungsten ore is crushed to granularity within the scope of 74 ~ 200 μm.
4. method according to claim 1, is characterized in that, described leaching carries out under temperature is the condition of 20 ~ 90 DEG C.
5. method according to claim 1, is characterized in that, fired slags adopts Na
2cO
3solution is crushed to granularity within the scope of 0.1mm ~ 1mm before leaching.
6. the method according to any one of Claims 1 to 5, is characterized in that, described sodium tungstate solution extracts tungsten by ion-exchange or extracting process.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410734362.3A CN104372169B (en) | 2014-12-04 | 2014-12-04 | Method of extracting tungsten from high-barium tungsten ore |
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|---|---|---|---|
| CN201410734362.3A CN104372169B (en) | 2014-12-04 | 2014-12-04 | Method of extracting tungsten from high-barium tungsten ore |
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|---|---|
| CN104372169A true CN104372169A (en) | 2015-02-25 |
| CN104372169B CN104372169B (en) | 2017-02-22 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293556A (en) * | 2015-10-12 | 2016-02-03 | 中南大学 | Method for extracting tungsten from tungsten-containing sodium carbonate solution and comprehensively utilizing extracted solution |
| CN105296749A (en) * | 2015-10-29 | 2016-02-03 | 江西稀有稀土金属钨业集团有限公司 | Method and system for dissolving barium-containing tungsten ores |
| CN106011504A (en) * | 2016-07-05 | 2016-10-12 | 江西理工大学 | Method for resolving scheelite |
| 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 |
| CN109468453A (en) * | 2018-12-14 | 2019-03-15 | 中南大学 | A method of tungsten being extracted from tungstenic raw material using cullet |
| CN111057880A (en) * | 2019-12-27 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| WO2020174907A1 (en) * | 2019-02-25 | 2020-09-03 | 三菱マテリアル株式会社 | Tungsten recovery method |
| CN114381618A (en) * | 2022-01-17 | 2022-04-22 | 江西理工大学 | Method for smelting tungsten ore |
| CN115072927A (en) * | 2022-08-01 | 2022-09-20 | 中南大学 | Method for recovering tungsten from tungsten smelting wastewater |
-
2014
- 2014-12-04 CN CN201410734362.3A patent/CN104372169B/en not_active Expired - Fee Related
Non-Patent Citations (2)
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| R.K.PARAMGURU等: ""用纯碱焙烧-浸出法从白钨精矿中提取钨"", 《湿法冶金》 * |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293556A (en) * | 2015-10-12 | 2016-02-03 | 中南大学 | Method for extracting tungsten from tungsten-containing sodium carbonate solution and comprehensively utilizing extracted solution |
| CN105296749A (en) * | 2015-10-29 | 2016-02-03 | 江西稀有稀土金属钨业集团有限公司 | Method and system for dissolving barium-containing tungsten ores |
| CN106011504A (en) * | 2016-07-05 | 2016-10-12 | 江西理工大学 | Method for resolving scheelite |
| 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 |
| CN109468453A (en) * | 2018-12-14 | 2019-03-15 | 中南大学 | A method of tungsten being extracted from tungstenic raw material using cullet |
| WO2020174907A1 (en) * | 2019-02-25 | 2020-09-03 | 三菱マテリアル株式会社 | Tungsten recovery method |
| CN111057880A (en) * | 2019-12-27 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| CN114381618A (en) * | 2022-01-17 | 2022-04-22 | 江西理工大学 | Method for smelting tungsten ore |
| CN115072927A (en) * | 2022-08-01 | 2022-09-20 | 中南大学 | Method for recovering tungsten from tungsten smelting wastewater |
| CN115072927B (en) * | 2022-08-01 | 2023-06-09 | 中南大学 | Method for recycling tungsten from tungsten smelting wastewater |
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| CN104372169B (en) | 2017-02-22 |
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Granted publication date: 20170222 Termination date: 20211204 |