CN106868321B - A method of processing scheelite extracts tungsten - Google Patents
A method of processing scheelite extracts tungsten Download PDFInfo
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- CN106868321B CN106868321B CN201710171219.1A CN201710171219A CN106868321B CN 106868321 B CN106868321 B CN 106868321B CN 201710171219 A CN201710171219 A CN 201710171219A CN 106868321 B CN106868321 B CN 106868321B
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- scheelite
- tungsten
- obtains
- roasting
- extraction
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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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- 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
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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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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of methods that processing scheelite extracts tungsten, and in particular to a kind of method of sodium hydroxide joint silica roasting scheelite extraction tungsten includes the following steps:Scheelite granularity is ground to less than 200 mesh by step 1；Step 2, by the scheelite and solid NaOH and SiO after grinding2It is uniformly mixed；The mixture that step 2 obtains is placed in high temperature kiln roasting by step 3；Step 4 carries out water logging to the calcining matter that step 3 obtains and obtains sodium tungstate solution.The method that sodium hydroxide of the present invention carries tungsten with silica mixed decomposition scheelite, overcome prior art using existing for autoclave produce intermittently operated, have the problem of certain security risk, simultaneously, compared with the sodium carbonate sintering process Decomposition of Tungsten of early stage, reaction temperature is nearly 200 DEG C low, tungsten recovery rate improves about 5%, greatly reduces energy consumption and improves the utilization rate of valuable tungsten resource.
Description
Technical field
The present invention relates to mineral manufacture field more particularly to a kind of methods for extracting tungsten from scheelite.
Background technology
The tungsten resource in the whole world nearly 70% is made of scheelite.Currently, with the continuous exhaustion of wolframite resource, scheelite is
Become the main raw material of industry.
Past, the common method for decomposing scheelite mainly have soda pressuring cooking method, hydrochloric acid leaching process and soda sintered method, by
In there are respective deficiency, it has been eliminated.In the 1980s, as Central South University professor Li Honggui develops alkali hot-bulb mill
Technique changes the view and caustic digestion scheelite of " can not possibly handle scheelite with NaOH decomposition methods in industrial conditions "
Theoretical and technique is gradually ripe and progressive, and making scheelite basic pressure digestion technique gradually becomes the prevailing technology of Tungsten smelting industry, currently,
The Tungsten smelting enterprise in the whole nation nearly 95% or more is all made of the production breakdown scheelite.But the equipment that the method uses still belongs to for autoclave
High-tension apparatus needs the decomposition that just can guarantee scheelite with 8-15 kilograms of pressure, and there are some potential safety problemss, meanwhile, production
Process operates for intermittent one-pot, and the scale and efficiency of production are by certain restriction.Therefore, be badly in need of developing new safety,
Continuously, efficient tungsten ore decomposition technique.
In fact, China's first generation Tungsten smelting production technology-sodium carbonate sintering process, can be in 800-900 DEG C of condition of sintering temperature
Lower continuous decomposition scheelite can meet above-mentioned requirements in form, but the problem of several keys needs to solve.It is well known that
Sodium carbonate sintering process is used for smelting wolframite earliest, is also applied for processing scheelite, but when handling scheelite, react generation
Calcium silicates and energy and Na2WO4It carries out secondary response and generates CaWO4, it is only 95% or so to cause tungsten ore resolution ratio, and be will produce big
The CO of amount2Greenhouse gases（《Non-ferrous extractive metallurgy handbook》Editorial board non-ferrous extractive metallurgies handbook-rare high-melting-point
Metal（On）The Beijing [M]：Metallurgical industry publishing house, 2005:88-95）, therefore, decomposing scheelite using roasting method needs further
The resolution ratio of tungsten ore is improved, while solving CO2The generation of gas.
Invention content
The purpose of the present invention is to provide a kind of use scope is wide, low energy consumption, and resolution ratio is high, the hydrogen-oxygen of low production cost
Change the method that sodium carries tungsten with silica mixed decomposition scheelite.
To achieve the above object, the present invention provides a kind of method that processing scheelite extracts tungsten, include the following steps.
Scheelite granularity is ground to less than 200 mesh by step 1.
Step 2, by the scheelite and solid NaOH and SiO after grinding2It is uniformly mixed.
The mixture that step 2 obtains is placed in high temperature kiln roasting by step 3.
Step 4 carries out water logging to the calcining matter that step 3 obtains and obtains sodium tungstate solution.
Further, with WO3Meter, in the scheelite 30~70wt. of tungstenic %, NaOH dosages be theoretical amount 1.0~
3.0 times, SiO2Dosage is 1.0-1.5 times of theoretical amount.
Further, in the step 3, at 600 ~ 800 DEG C, roasting time is controlled 1.0 ~ 3.0 for calcination temperature control
Hour.
Further, in the step 4, the liquid-solid ratio of leaching is 2:1~5:1；Extraction temperature is controlled in room temperature to 95
DEG C, extraction time was controlled at 3.0 ~ 5.0 hours.
Further, extraction temperature control is at 50 ~ 80 DEG C.
The beneficial effects of the invention are as follows：Sodium hydroxide of the present invention carries tungsten with silica mixed decomposition scheelite
Method, by reacting scheelite with the baking mixed realization of solid sodium hydroxide and silica；Compared with the prior art, overcome
Using producing intermittently operated existing for autoclave, have the problem of certain security risk, meanwhile, sodium carbonate sintering process with early stage
Decomposition of Tungsten is compared, and reaction temperature is nearly 200 DEG C low, and tungsten recovery rate improves about 5%, is greatly reduced energy consumption and is improved valuable tungsten
The utilization rate of resource.
Description of the drawings
Fig. 1 is the process flow chart for the method that processing scheelite provided by the invention extracts tungsten.
Fig. 2 is the XRD analysis detection figure of product of roasting in the present invention.
Specific implementation mode
As long as decomposing the classical theory of scheelite by sodium hydroxide --- counterfeit ternary phase diagrams is it is found that the concentration of sodium hydroxide is sufficient
Enough height, can decompose scheelite under conditions of normal temperature and pressure, if improving the concentration of sodium hydroxide to ultimate attainment, i.e. solid hydrogen
Sodium oxide molybdena, while mixing certain temperature, if scheelite is equally decomposed, the side of sodium hydroxide Roasting Decomposition scheelite is formed
Method.Based on this imagination, seminar is placed in after white tungsten fine ore and sodium hydroxide batch mixing in corundum crucible and is roasted, as a result sent out
Existing slag tungstenic is 3.88%, as a result unsatisfactory；And same dispensing is pressed, it is placed in ceramic crucible, and roasted by same condition
When burning, slag tungstenic is only 0.25%, excellent.The difference of two experiments is only crucible material, by examination, two kinds of crucible materials
SiO in matter2Content ceramic crucible is far above corundum crucible.Therefore, according to identical white tungsten fine ore and sodium hydroxide charge ratio, together
When a certain amount of SiO is added2, it is placed in corundum crucible, is roasted under identical roasting condition, slag tungstenic is 0.28%, is further proved
SiO2Effect during sodium hydroxide Roasting Decomposition scheelite, product of roasting are detected as Na by XRD analysis2CaSiO4
（Na2O·CaO·SiO2）, it is a kind of new ternary slag rather than the calcium silicates that soda sintered method generates, it is anti-is inferred to this as a result,
The equation answered is as follows.
CaWO4+4NaOH+SiO2=Na2WO4+Na2CaSiO4+2H2O
It is found based on the studies above, the present invention proposes a kind of sodium hydroxide and carries tungsten with silica mixed decomposition scheelite
Method the present invention is further described below in conjunction with the accompanying drawings in order to more clearly state the present invention.
Refering to fig. 1, the method that sodium hydroxide provided by the invention carries tungsten with silica mixed decomposition scheelite, changes
The technique for decomposing scheelite with NaOH solution in the prior art, uses NaOH solids and SiO instead2Solid roasting decomposes scheelite.
Specifically, include the following steps.
Scheelite granularity is ground to less than 200 mesh, with WO by step 13It counts, 30~70wt. of tungstenic in the scheelite
%。
Step 2, by the scheelite and solid NaOH and SiO after grinding2It is uniformly mixed, NaOH dosages are the 1.0 of theoretical amount
~3.0 times, SiO2Dosage is 1.0-1.5 times of theoretical amount.
The mixture that step 2 obtains is placed in high temperature kiln roasting by step 3；Calcination temperature is controlled at 600 ~ 800 DEG C,
Roasting time was controlled at 1.0 ~ 3.0 hours.
Step 4, the calcining matter obtained to step 3 carry out water logging and obtain sodium tungstate solution, wherein the liquid-solid ratio of leaching is
2:1~5:1；In room temperature to 95 DEG C, extraction time was controlled at 3.0 ~ 5.0 hours for extraction temperature control.It is preferred that the extraction temperature
Control is at 50 ~ 80 DEG C.
It is more specific embodiment below.
Embodiment 1：Certain white tungsten fine ore contains 62.45%WO3, granularity is -200 mesh.Mine weight 100g, 2.0 times of theory NaOH use
Amount, 1 times of theory SiO2Dosage, 700 DEG C of roasting 2.0h, product of roasting add water leaching, liquid-solid ratio 5:1, temperature 70 C, heat preservation
3h is filtered, and is washed, drying, contains insoluble WO in slag3It is 0.26%, resolution ratio is up to 99.78%.
Embodiment 2：Contain 46.77%WO in certain scheelite3, granularity is -250 mesh.Mine weight 80g, 2.5 times of theory NaOH dosages,
1.3 times of theory SiO2Dosage, 800 DEG C of roasting 3h, product of roasting add water leaching, liquid-solid ratio 4:1, temperature 50 C keeps the temperature 4h,
Filtering is washed, drying, contains insoluble WO in slag3It is 0.21%, resolution ratio is up to 99.85%.
Embodiment 3：Contain 52.36%WO in certain scheelite3, granularity is -250 mesh.Take above-mentioned mine 150g, 1.5 times of theory NaOH
Dosage, 1.2 times of theory SiO2Dosage, 600 DEG C of roasting 1h, product of roasting add water leaching, liquid-solid ratio 2:1, temperature is room
Temperature keeps the temperature 3.5h, filters, and washes, drying, contains insoluble WO in slag3It is 8.48%, resolution ratio is up to 93.76%.
Embodiment 4：Contain 35.71%WO in certain scheelite3, granularity is -300 mesh.Mine weight 200g, 1.3 times of theory NaOH use
Amount, 1.5 times of theory SiO2Dosage, 650 DEG C of roasting 3h, product of roasting add water leaching, liquid-solid ratio 3:1,80 DEG C of temperature, heat preservation
5h is filtered, and is washed, drying, contains insoluble WO in slag3It is 0.33%, resolution ratio is up to 98.64%.
It can be obtained from above-mentioned test data, sodium hydroxide of the invention carries tungsten with silica mixed decomposition scheelite
Method, can the arbitrary scheelite of efficient-decomposition, compared with existing alkali decomposition process, overcome using existing for autoclave produce interval
It operates, have the problem of certain security risk, meanwhile, compared with the sodium carbonate sintering process Decomposition of Tungsten of early stage, reaction temperature is low close
200 DEG C, tungsten recovery rate improves about 5%, greatly reduces energy consumption and improves the utilization rate of valuable tungsten resource.
It these are only the preferred embodiment of the present invention, it is noted that those skilled in the art are come
It says, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of method of processing scheelite extraction tungsten, which is characterized in that include the following steps：
Scheelite granularity is ground to less than 200 mesh by step 1；
Step 2, by the scheelite and solid NaOH and SiO after grinding2It is uniformly mixed, NaOH dosages are the 1.0~3.0 of theoretical amount
Times, SiO2Dosage is 1.0-1.5 times of theoretical amount；
The mixture that step 2 obtains is placed in high temperature kiln roasting by step 3；
Step 4 carries out water logging to the calcining matter that step 3 obtains and obtains sodium tungstate solution.
2. the method for processing scheelite extraction tungsten according to claim 1, which is characterized in that with WO3Meter, the scheelite
Middle 30~70wt. of tungstenic %.
3. handling the method that scheelite extracts tungsten according to claim 1-2 any one of them, which is characterized in that in the step
In three, at 600 ~ 800 DEG C, roasting time was controlled at 1.0 ~ 3.0 hours for calcination temperature control.
4. handling the method that scheelite extracts tungsten according to claim 1-2 any one of them, which is characterized in that in the step
In four, the liquid-solid ratio of leaching is 2:1~5:1；In room temperature to 95 DEG C, extraction time control is small 3.0 ~ 5.0 for extraction temperature control
When.
5. handling the method that scheelite extracts tungsten according to claim 1-2 any one of them, which is characterized in that in the step
In four, the liquid-solid ratio of leaching is 2:1~5:1；At 50 ~ 80 DEG C, extraction time was controlled at 3.0 ~ 5.0 hours for extraction temperature control.
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| CN109468453B (en) * | 2018-12-14 | 2020-09-11 | 中南大学 | Method for extracting tungsten from tungsten-containing raw material by using waste glass |
| CN115353148A (en) * | 2022-08-31 | 2022-11-18 | 赣州有色冶金研究所有限公司 | Method for recovering sodium hydroxide from sodium tungstate alkali cooking liquor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011017A (en) * | 2010-11-19 | 2011-04-13 | 中南大学 | Method for extracting tungsten by decomposing tungsten minerals |
| CN104789772A (en) * | 2015-04-06 | 2015-07-22 | 桂林理工大学 | Energy-saving and consumption-reducing method for alkaline leaching of scheelite |
| CN105112691A (en) * | 2015-10-10 | 2015-12-02 | 江西理工大学 | Method for extracting tungsten from tungsten minerals through alkaline decomposition |
| CN105969977A (en) * | 2016-07-05 | 2016-09-28 | 江西理工大学 | Method for extracting tungsten from scheelite |
| CN106011504A (en) * | 2016-07-05 | 2016-10-12 | 江西理工大学 | Method for resolving scheelite |
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- 2017-03-21 CN CN201710171219.1A patent/CN106868321B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011017A (en) * | 2010-11-19 | 2011-04-13 | 中南大学 | Method for extracting tungsten by decomposing tungsten minerals |
| CN104789772A (en) * | 2015-04-06 | 2015-07-22 | 桂林理工大学 | Energy-saving and consumption-reducing method for alkaline leaching of scheelite |
| CN105112691A (en) * | 2015-10-10 | 2015-12-02 | 江西理工大学 | Method for extracting tungsten from tungsten minerals through alkaline decomposition |
| CN105969977A (en) * | 2016-07-05 | 2016-09-28 | 江西理工大学 | Method for extracting tungsten from scheelite |
| CN106011504A (en) * | 2016-07-05 | 2016-10-12 | 江西理工大学 | Method for resolving scheelite |
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