CN113106251A - Chemical beneficiation method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore - Google Patents
Chemical beneficiation method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore Download PDFInfo
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- CN113106251A CN113106251A CN202110259045.0A CN202110259045A CN113106251A CN 113106251 A CN113106251 A CN 113106251A CN 202110259045 A CN202110259045 A CN 202110259045A CN 113106251 A CN113106251 A CN 113106251A
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- tin
- wolframite
- acid solution
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- middlings
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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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
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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
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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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet 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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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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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- Metallurgy (AREA)
- Mechanical Engineering (AREA)
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- Environmental & Geological Engineering (AREA)
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- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a chemical beneficiation method for producing tin middling from high-tin wolframite or mixed wolframite and scheelite, which comprises the steps of adding the high-tin wolframite or mixed wolframite and scheelite into a hydrochloric acid solution, stirring for reaction, and carrying out solid-liquid separation to obtain washing liquor and filter residue; and (2) adding the filter residue obtained in the step (1) into a phosphoric acid solution, stirring for reaction, and filtering to obtain tin middlings with the Sn content of 5-15% and filtrate. The method realizes effective separation of tungsten and tin in the high-tin tungsten mineral, greatly reduces the tin removal pressure in the tungsten smelting process, and simultaneously produces the tin middlings which can be used as raw materials for volatilizing and extracting tin in a fuming furnace, thereby realizing resource utilization of tin and having remarkable economic benefit.
Description
Technical Field
The invention belongs to extraction of associated metallic tin, and particularly relates to a chemical beneficiation method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore.
Background
China is a large country of tungsten resources, particularly in south China, large hydrothermal quartz vein-type ore deposits contain a large amount of tungsten and are accompanied by metals such as tin, bismuth and the like, and belong to typical multi-metal mineral deposits, most typically large-scale-ultra-large tungsten-tin multi-metal ore deposits such as persimmon bamboo gardens, new fields, west China and the like. At present, the ores are mainly separated by flotation-gravity separation-magnetic separation technology, sulfide ores are produced by flotation, flotation tailings are subjected to gravity separation to recover wolframite and stannum, and finally, tungsten and tin are separated by strong magnetic separation. The ore pulp amount of the ore dressing operation method is large, the medicament consumption is large, the production cost is high, and more outstanding problems are that the symbiotic relationship of tungsten and tin is complex, the mineral embedding granularity is fine, so that tungsten and tin are not completely separated, a considerable part of tin enters tungsten concentrate in an impurity form, and the Sn content in the tungsten concentrate can reach about 1.5 percent. For a long time, tin cannot be recycled in the tungsten smelting process, so that the waste of tin resources is caused. When the content of tin in the tungsten concentrate is high, a special tin removing procedure is needed in the tungsten smelting process, otherwise, the content of tin in the tungsten product exceeds the standard, and the quality of the tungsten product is seriously influenced.
Disclosure of Invention
In order to overcome the defects in the prior art and solve the problem that the prior art is difficult to recycle associated tin resources, the invention provides a chemical beneficiation method for producing tin middlings from high-tin wolframite or wolframite mixed ore, so that the high-efficiency separation of tin and tungsten is realized, the tin middlings with the produced Sn content of 5-15% can be used as raw materials for volatilizing and extracting tin in a fuming furnace, the recycling of the associated tin resources in tungsten concentrate is realized, and the economic benefit is remarkable.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a chemical ore dressing method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore comprises the following steps:
(1) adding high-tin wolframite or wolframite and wolframite mixed ore into a hydrochloric acid solution, stirring for reaction, and carrying out solid-liquid separation to obtain washing liquid and filter residue;
(2) and (2) adding the filter residue obtained in the step (1) into a phosphoric acid solution, stirring for reaction, and filtering to obtain tin middlings with the Sn content of 5-15% and filtrate.
Preferably, in the step (1), the Sn content in the high-tin wolframite or the wolframite-wolframite mixed ore is 0.5-1.5 wt%.
Preferably, in the step (1), the liquid-solid ratio of the hydrochloric acid solution to the high-tin wolframite or wolframite mixed ore is 1-5 ml:1g, and the concentration of the hydrochloric acid solution is 150-250 g/L.
Preferably, in the step (1), the stirring reaction is carried out at the temperature of 25-70 ℃ for 1-5 hours.
Preferably, in the step (2), the liquid-solid ratio of the phosphoric acid solution to the filter residue is 1-5 ml:1g, and the concentration of the phosphoric acid solution is 10-50 g/L.
Preferably, in the step (2), the stirring reaction is carried out at the temperature of 70-90 ℃ for 1-5 hours.
The invention has the advantages that:
the method realizes effective separation of tungsten and tin in the high-tin tungsten mineral, greatly reduces the tin removal pressure in the tungsten smelting process, and simultaneously produces the tin middlings which can be used as raw materials for volatilizing and extracting tin in a fuming furnace, thereby realizing resource utilization of tin and having remarkable economic benefit.
Detailed Description
In order to explain the present invention in more detail, the following examples are given for illustration, but the present invention is not limited to these examples.
Example 1
Adding high-tin wolframite with the Sn content of 0.5 wt% into 150g/L hydrochloric acid solution according to the liquid-solid ratio of 1ml to 1g, stirring and reacting for 5 hours at 50 ℃, and carrying out solid-liquid separation to obtain washing liquid and filter residue; adding the filter residue into 30g/L phosphoric acid according to the liquid-solid ratio of 1ml to 1g, stirring and reacting for 2h at 90 ℃, filtering to obtain tin middlings with the Sn content of 5.28 wt% and filtrate, and recycling the obtained filtrate as a raw material for extracting tungsten or supplementing phosphoric acid.
Example 2
Adding high-tin wolframite and wolframite mixed ore with the Sn content of 1.2 wt% into 200g/L hydrochloric acid solution according to the liquid-solid ratio of 5ml to 1g, stirring and reacting for 3h at 25 ℃, and obtaining washing liquid and filter residue after solid-liquid separation; adding the filter residue into 10g/L phosphoric acid according to the liquid-solid ratio of 3ml to 1g, stirring and reacting for 3h at 80 ℃, filtering to obtain tin middlings with the Sn content of 12.65 wt% and filtrate, and recycling the obtained filtrate as a raw material for extracting tungsten or supplementing phosphoric acid.
Example 3
Adding high-tin wolframite with the Sn content of 1.5 wt% into 250g/L hydrochloric acid solution according to the liquid-solid ratio of 3ml to 1g, stirring and reacting for 1h at 70 ℃, and carrying out solid-liquid separation to obtain washing liquid and filter residue; adding the filter residue into 50g/L phosphoric acid according to the liquid-solid ratio of 2ml to 1g, stirring and reacting for 1h at 90 ℃, filtering to obtain tin middlings with the Sn content of 14.72 wt% and filtrate, and recycling the obtained filtrate as a raw material for extracting tungsten or supplementing phosphoric acid.
Example 4
Adding high-tin wolframite and wolframite mixed ore with the Sn content of 0.85 wt% into 200g/L hydrochloric acid solution according to the liquid-solid ratio of 2ml to 1g, stirring and reacting for 4 hours at 50 ℃, and obtaining washing liquid and filter residue after solid-liquid separation; adding the filter residue into 30g/L phosphoric acid according to the liquid-solid ratio of 5ml to 1g, stirring and reacting for 2h at 90 ℃, filtering to obtain tin middlings with 9.28 wt% of Sn content and filtrate, and recycling the obtained filtrate as a raw material for extracting tungsten or supplementing phosphoric acid.
Example 5
Adding high-tin wolframite and wolframite mixed ore with the Sn content of 1.2 wt% into 200g/L hydrochloric acid solution according to the liquid-solid ratio of 1ml to 1g, stirring and reacting for 3h at 50 ℃, and obtaining washing liquid and filter residue after solid-liquid separation; adding the filter residue into 50g/L phosphoric acid according to the liquid-solid ratio of 1ml to 1g, stirring and reacting for 5h at 70 ℃, filtering to obtain tin middlings with 13.86 wt% of Sn content and filtrate, and recycling the obtained filtrate as a raw material for extracting tungsten or supplementing phosphoric acid.
Claims (6)
1. A chemical ore dressing method for producing tin middling from high-tin wolframite or wolframite-wolframite mixed ore is characterized by comprising the following steps:
(1) adding high-tin wolframite or wolframite and wolframite mixed ore into a hydrochloric acid solution, stirring for reaction, and carrying out solid-liquid separation to obtain washing liquid and filter residue;
(2) and (2) adding the filter residue obtained in the step (1) into a phosphoric acid solution, stirring for reaction, and filtering to obtain tin middlings with the Sn content of 5-15% and filtrate.
2. The chemical beneficiation process for producing tin middlings from high tin wolframite or mixed wolframite and scheelite ores according to claim 1, wherein: in the step (1), the Sn content in the high-tin wolframite or the wolframite-wolframite mixed ore is 0.5-1.5 wt%.
3. The chemical beneficiation process for producing tin middlings from high tin wolframite or mixed wolframite and scheelite ores according to claim 1, wherein: in the step (1), the liquid-solid ratio of the hydrochloric acid solution to the high-tin wolframite or wolframite mixed ore is 1-5 ml:1g, and the concentration of the hydrochloric acid solution is 150-250 g/L.
4. The chemical beneficiation process for producing tin middlings from high tin wolframite or mixed wolframite and scheelite ores according to claim 1, wherein: in the step (1), the stirring reaction is carried out at the temperature of 25-70 ℃ for 1-5 h.
5. The chemical beneficiation process for producing tin middlings from high tin wolframite or mixed wolframite and scheelite ores according to claim 1, wherein: in the step (2), the liquid-solid ratio of the phosphoric acid solution to the filter residue is 1-5 ml:1g, and the concentration of the phosphoric acid solution is 10-50 g/L.
6. The chemical beneficiation process for producing tin middlings from high tin wolframite or mixed wolframite and scheelite ores according to claim 1, wherein: in the step (2), the stirring reaction is carried out at the temperature of 70-90 ℃ for 1-5 h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110259045.0A CN113106251B (en) | 2021-03-10 | 2021-03-10 | Chemical beneficiation method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore |
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| CN202110259045.0A CN113106251B (en) | 2021-03-10 | 2021-03-10 | Chemical beneficiation method for producing tin middling from high-tin wolframite or wolframite and wolframite mixed ore |
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| CN113106251A true CN113106251A (en) | 2021-07-13 |
| CN113106251B CN113106251B (en) | 2023-03-10 |
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| CN102021329A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite and producing high-quality calcined gypsum |
| CN102021327A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for decomposing scheelite by using phosphoric acid |
| CN102021328A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite |
| CN102080157A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for decomposing scheelite |
| CN102080161A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for comprehensively recovering tungsten and phosphorus from high phosphorus white tungsten ores |
| CN108642308A (en) * | 2018-04-13 | 2018-10-12 | 中南大学 | A kind of method that high tin tungsten ore is decomposed in mixture of sulfuric phosphoric acid pressurization |
| CN109092564A (en) * | 2018-06-29 | 2018-12-28 | 湖南柿竹园有色金属有限责任公司 | A kind of beneficiation method of black and white tungsten tin bulk concentrate |
| CN110004294A (en) * | 2019-03-04 | 2019-07-12 | 中南大学 | The processing method of scheelite caustic digestion slag |
| CN110038727A (en) * | 2019-04-19 | 2019-07-23 | 北京矿冶科技集团有限公司 | A kind of separation method of white tungsten tin bulk concentrate |
| US20200190627A1 (en) * | 2018-12-18 | 2020-06-18 | Jiangxi University Of Science And Technology | Method for decomposing medium-/low-grade scheelite |
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2021
- 2021-03-10 CN CN202110259045.0A patent/CN113106251B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2221887C1 (en) * | 2002-06-18 | 2004-01-20 | Орловский государственный технический университет | Method of processing compound tungsten-tin concentrates |
| CN102021329A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite and producing high-quality calcined gypsum |
| CN102021327A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for decomposing scheelite by using phosphoric acid |
| CN102021328A (en) * | 2010-12-24 | 2011-04-20 | 中南大学 | Method for extracting tungsten from scheelite |
| CN102080157A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for decomposing scheelite |
| CN102080161A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for comprehensively recovering tungsten and phosphorus from high phosphorus white tungsten ores |
| CN108642308A (en) * | 2018-04-13 | 2018-10-12 | 中南大学 | A kind of method that high tin tungsten ore is decomposed in mixture of sulfuric phosphoric acid pressurization |
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| CN110004294A (en) * | 2019-03-04 | 2019-07-12 | 中南大学 | The processing method of scheelite caustic digestion slag |
| CN110038727A (en) * | 2019-04-19 | 2019-07-23 | 北京矿冶科技集团有限公司 | A kind of separation method of white tungsten tin bulk concentrate |
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