CN108179270A - A kind of method of silicone content in reduction sodium tungstate solution - Google Patents
A kind of method of silicone content in reduction sodium tungstate solution Download PDFInfo
- Publication number
- CN108179270A CN108179270A CN201711363476.1A CN201711363476A CN108179270A CN 108179270 A CN108179270 A CN 108179270A CN 201711363476 A CN201711363476 A CN 201711363476A CN 108179270 A CN108179270 A CN 108179270A
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- CN
- China
- Prior art keywords
- solution
- content
- sodium tungstate
- silicone content
- sodium
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Classifications
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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
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
-
- 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
-
- 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
Abstract
A kind of method for reducing silicone content in sodium tungstate solution of the present invention, by adding aluminium salt in soda pressuring cooking scheelite process, silicon is in the form of silicic acid as autoclaving slag is discharged, one outlet is found for impurity such as silicon, reduce the enrichment in alkaline extraction section, play the role of reducing silicone content in sodium tungstate solution, ensure the normal operation of alkaline extraction, be suitble to large-scale promotion and application.
Description
【Technical field】
The present invention relates to a kind of methods for reducing silicone content in sodium tungstate solution, and in particular to a kind of soda pressuring cooking decomposes tungsten concentrate
The method of silicone content in the sodium tungstate solution of generation.
【Background technology】
Soda (alkali) autoclaving that Wu Ye companies of Luo Mu groups use-alkaline extraction process scheelite complete set technology is for processing
The customization of Lip river molybdenum low-grade scheelite, which there is leaching-extract to be recycled to be closed flow, water and alkali, anacidity disappears
Consumption, the tungsten loss waste water that tungsten loss, the no removing impurity by means of precipitation that theoretical alkaline consumption is zero, no water phase open circuit is brought are brought can accomplish zero
Discharge, generated without dangerous solid waste phosphorus and arsenic slag, technological process it is short, tungsten yield improves, production cost is greatly lowered, product quality height etc.
Advantage.But since the system is is closed flow, with production more than a year, using the impurity that silicon is representative when alkali extracts and extracts segment length
Between enrichment form indissoluble floccule, influence normal split-phase, cause production difficult, be detected as silicon and be precipitated when PH is less than 9.5, it is special
It is not 7 grades and 8 grades of alkaline extraction, analysis reason is high for silicone content in sodium tungstate solution, into alkaline extraction system, alkaline extraction
8 grades are blank organic phases（PH value is 8）Basicity reduction causes the impurity such as silicic acid to be precipitated when being mixed with alkali extraction raffinate.So
How a kind of method that reduces in sodium tungstate solution silicone content is provided just into the long-term technology demand of those skilled in the art.
【Invention content】
It is insufficient to overcome present in background technology, the present invention provides a kind of method for reducing silicone content in sodium tungstate solution,
By adding in a kind of aluminium salt in decomposing scheelite process in soda pressuring cooking, aluminium salt is by hydrolysis generation aluminium hydroxide, aluminium hydroxide
The solubility of silicic acid in solution is carried and reduced by absorption, and silicic acid is made to be discharged together with precipitation and soda pressuring cooking slag, thus
Achieve the purpose that reduce silicone content in sodium tungstate solution.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of method of silicone content in reduction sodium tungstate solution, the method in dosage bunker add in sodium carbonate aqueous solution,
Scheelite, magnesium salts and aluminium salt are deployed into ore pulp, and control liquor capacity is 75% or so of dosage bunker volume, carbonic acid in solution at this time
Sodium content is in 160 ~ 200g/l, and sodium hydrate content is in 0 ~ 6g/l, and magnesium salts content is in 7 ~ 11g/l, and aluminium salt content is in 2 ~ 4g/l.It will
Deployed ore pulp is transferred in high pressure leaching kettle, and scheelite is decomposed under high-temperature and high-pressure conditions generates sodium tungstate solution.Add aluminium
Silicone content can reduce by more than 80% in sodium tungstate solution after salt, and silicone content is down to 0.2g/l hereinafter, ensure that alkalinity in minimum system
The normal operation of extraction.
The method for reducing silicone content in sodium tungstate solution, the aqueous sodium carbonate liquid are with lime treatment alkalinity
Raffinate（Water phase after alkaline extraction）Solution afterwards.
The method for reducing silicone content in sodium tungstate solution, the additive amount of the magnesium salts is about scheelite weight
4.5%。
The method for reducing silicone content in sodium tungstate solution, the additive amount of the aluminium salt is about scheelite weight
1.5%。
The method for reducing silicone content in sodium tungstate solution, the aqueous sodium carbonate can be recycled.
The method for reducing silicone content in sodium tungstate solution extracts alkali for anion in reduction aluminium ion and aluminium salt
It influences, it is impossible to which long-term addition should monitor silicone content in sodium tungstate solution, according to circumstances add.
The described method for reducing silicone content in sodium tungstate solution, silicone content normal value should control in the sodium tungstate solution
In below 0.4g/l.
The method for reducing silicone content in sodium tungstate solution, belongs in Tungsten smelting industry and uses for the first time.
Using technical solution as described above, the present invention has superiority as described below：
For the present invention by adding aluminium salt in soda pressuring cooking scheelite process, silicon, as autoclaving slag is discharged, is silicon in the form of silicic acid
Impurity is waited to find one outlet, reduce the enrichment in alkaline extraction section, play the role of reducing silicone content in sodium tungstate solution,
Ensure the normal operation of alkaline extraction, be suitble to large-scale promotion and application.
【Description of the drawings】
Fig. 1 is the process flow chart of the present invention.
【Specific embodiment】
The present invention can be explained in more detail by the following examples, the invention is not limited in the following examples；
Alkali extraction rapid lapse of time is enriched with the indissoluble floccule to be formed first to be dissolved with liquid caustic soda, dissolved aqueous solution（It is alkali
Extract raffinate）With lime conversion processing, the sodium bicarbonate in solution is converted to sodium carbonate, and keep sodium hydrate content 0 ~
6g/l, then with this solution come washery slag, solution is known as causticization washing lotion after washery slag, with causticization washing lotion, magnesium salts, aluminium salt, scheelite tune
Be made into ore pulp, at this time in solution carbonate content in 160 ~ 200g/l, sodium hydrate content within 6g/l, magnesium salts content 7 ~
11g/l, aluminium salt content are transferred in high pressure leaching kettle in 2 ~ 4g/l, and scheelite is decomposed generation wolframic acid under high-temperature and high-pressure conditions
Sodium solution.By 1 month addition aluminium salt and magnesium salts experiment, solution ceaselessly recycles from soda pressuring cooking to alkaline extraction system,
High silicon solution is gradually replaced by low silicon solution, and silicone content has been down to 0.2g/l hereinafter, ensureing by highest 4.8g/l in system
The normal operation of alkaline extraction.
Part not in the detailed description of the invention is the prior art.
Claims (5)
- A kind of 1. method for reducing silicone content in sodium tungstate solution：It is characterized by comprising following steps：Alkali is extracted first Rapid lapse of time is enriched with the indissoluble floccule caustic lye of soda alkali soluble solution to be formed, and dissolved aqueous solution extracts raffinate, alkali alkali Extract raffinate lime conversion processing, the sodium bicarbonate in solution be converted to sodium carbonate, and keep sodium hydrate content 0 ~ Then 6g/l obtains causticization slag with this solution come washery slag, solution is known as causticization washing lotion after washery slag, with causticization washing lotion, magnesium salts, aluminium Salt, scheelite are deployed into ore pulp, and carbonate content will be maintained at 160 ~ 200g/l in solution at this time, and sodium hydrate content is maintained at Within 6g/l, magnesium salts content is maintained at 7 ~ 11g/l, and aluminium salt content is maintained at 2 ~ 4g/l, and ore pulp is transferred to high pressure after deployed soaks Go out in kettle, scheelite is decomposed into generation sodium tungstate solution under high-temperature and high-pressure conditions, washing is filtered with water later, after washing Filtrate extracted again, the solution after extraction continues to be converted with lime to form causticization washing lotion for allocating ore pulp.
- 2. a kind of method for reducing silicone content in sodium tungstate solution according to claim 1, it is characterised in that：It is described severe It is with the solution after lime treatment alkalinity raffinate to change washing lotion.
- 3. a kind of method for reducing silicone content in sodium tungstate solution according to claim 1, it is characterised in that：The magnesium salts Additive amount be scheelite weight 4.5%.
- 4. a kind of method for reducing silicone content in sodium tungstate solution according to claim 1, it is characterised in that：The aluminium salt Additive amount be scheelite weight 1.5%.
- 5. a kind of method for reducing silicone content in sodium tungstate solution according to claim 1, it is characterised in that：The wolframic acid Silicone content just needs to add aluminium salt in more than 0.4g/l in sodium solution.
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| CN201711363476.1A CN108179270A (en) | 2017-12-18 | 2017-12-18 | A kind of method of silicone content in reduction sodium tungstate solution |
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| CN201711363476.1A CN108179270A (en) | 2017-12-18 | 2017-12-18 | A kind of method of silicone content in reduction sodium tungstate solution |
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| CN108179270A true CN108179270A (en) | 2018-06-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109825725A (en) * | 2019-03-25 | 2019-05-31 | 湖南懋天世纪新材料有限公司 | A kind of method of comprehensive utilization of tungstenic causticization slag |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4311679A (en) * | 1981-01-19 | 1982-01-19 | Amax Inc. | Treatment of sodium tungstate leach liquor containing dissolved silica, phosphorus, and fluorine impurities |
| CN1210894A (en) * | 1996-04-02 | 1999-03-17 | 中南工业大学 | Producing pure tungsten compound using tungsten-containing material |
| CN101445275A (en) * | 2008-09-25 | 2009-06-03 | 中南大学 | Centrifugal extracting method for preparing ammonium tungstate solution from soda leach liquor of tungsten contained material |
| CN101880780A (en) * | 2010-06-04 | 2010-11-10 | 中南大学 | Method for separating and extracting tungsten-molybdenum from mixed solution of tungstate-molybdate |
| CN103572075A (en) * | 2013-10-15 | 2014-02-12 | 中南大学 | Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system |
| CN106430787A (en) * | 2016-10-25 | 2017-02-22 | 湖南懋天世纪新材料有限公司 | APT (ammonium paratungstate) production wastewater recycling method |
-
2017
- 2017-12-18 CN CN201711363476.1A patent/CN108179270A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4311679A (en) * | 1981-01-19 | 1982-01-19 | Amax Inc. | Treatment of sodium tungstate leach liquor containing dissolved silica, phosphorus, and fluorine impurities |
| CN1210894A (en) * | 1996-04-02 | 1999-03-17 | 中南工业大学 | Producing pure tungsten compound using tungsten-containing material |
| CN101445275A (en) * | 2008-09-25 | 2009-06-03 | 中南大学 | Centrifugal extracting method for preparing ammonium tungstate solution from soda leach liquor of tungsten contained material |
| CN101880780A (en) * | 2010-06-04 | 2010-11-10 | 中南大学 | Method for separating and extracting tungsten-molybdenum from mixed solution of tungstate-molybdate |
| CN103572075A (en) * | 2013-10-15 | 2014-02-12 | 中南大学 | Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system |
| CN106430787A (en) * | 2016-10-25 | 2017-02-22 | 湖南懋天世纪新材料有限公司 | APT (ammonium paratungstate) production wastewater recycling method |
Non-Patent Citations (2)
| Title |
|---|
| GUIQING ZHANG ET AL: "A novel process for tungsten hydrometallurgy based on direct solvent extraction in alkaline medium", 《HYDROMETALLURGY》 * |
| 张启修等: "《萃取冶金原理与实践》", 31 August 2014, 中南大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109825725A (en) * | 2019-03-25 | 2019-05-31 | 湖南懋天世纪新材料有限公司 | A kind of method of comprehensive utilization of tungstenic causticization slag |
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Application publication date: 20180619 |