CN109306403A - The processing method of quaternary ammonium salt alkaline extraction three-phase flocculate in tungsten hydrometallurgy - Google Patents

The processing method of quaternary ammonium salt alkaline extraction three-phase flocculate in tungsten hydrometallurgy Download PDF

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Publication number
CN109306403A
CN109306403A CN201811262449.XA CN201811262449A CN109306403A CN 109306403 A CN109306403 A CN 109306403A CN 201811262449 A CN201811262449 A CN 201811262449A CN 109306403 A CN109306403 A CN 109306403A
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phase
flocculate
tungsten
extraction
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CN109306403B (en
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赵玲平
雷吟春
曹育龙
蒋纯
李湘军
龙扬
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Hunan Maotian Shijie New Materials Co Ltd
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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
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/28—Amines
    • C22B3/288—Quaternary ammonium
    • 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

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The processing method of quaternary ammonium salt alkaline extraction three-phase flocculate in tungsten hydrometallurgy.The present invention relates to the methods that the three-phase flocculate that a kind of pair of tungsten alkaline extraction generates is handled, the method includes the processes such as being mixed to three-phase flocculate, stir, heat, keep the temperature using lime, it is demulsified to three-phase flocculate, consequently facilitating being post-processed, filter residue after carrying out filters pressing is added roasting material as additive after diaphragm pressing and is sintered recycling tungsten therein, water phase returns to production line, and organic phase returns to extraction line, to realize the recycling to material.

Description

The processing method of quaternary ammonium salt alkaline extraction three-phase flocculate in tungsten hydrometallurgy
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to for quaternary ammonium salt alkaline extraction in tungsten hydrometallurgy The improved method that three-phase flocculate is handled.
Background technique
In tungsten metallurgy, sodium carbonate or sodium hydroxide alkali soaking technology Decomposition of Tungsten are mostly used greatly, it is straight from alkaline medium The new process for connecing extraction tungsten can solve ion exchange and acid extract technique problem encountered, can effectively remove while transition The impurity such as P, As, Si are removed, without adjusting acid and dilution, have that process is short, alkaline consumption is low, water consume is low and excellent without a large amount of waste water containing sodium etc. Point, therefore be a kind of tungsten hydrometallurgy cleaning procedure of great prospects for commercial application.Since the 1960s, domestic and foreign scholars A series of researchs are just carried out to this, American scholar Drobnick J L and Lewis C J, which has been investigated, uses quaternary ammonium salt from CO3 2-'s The rule of tungsten is extracted in sodium tungstate solution, in the 1990s, Zhang Guiqing etc. uses domestic quaternary ammonium salt N263+ sec-octyl alcohol+sulfonation Kerosene directly extracts tungsten from tungsten ore leaching with sodium hydroxide liquid, with NH4HCO3For stripping agent, realized in the experimental study stage Decontamination P, As, Si out while tungsten makes the transition.However, selected extraction system exists, extraction split-phase performance is poor, and gravity split-phase is fast (Ke Zhaohua etc., quaternary ammonium salt extract the problems such as degree is slower, and subsequent evaporation crystallization and evaporation amount is big, energy consumption is high from alkaline sodium tungstate solution Take the research of tungsten).
Using quaternary amine N263 (tri-n-octyl methyl ammonium chloride), direct tungsten makes the transition under alkaline condition and the technique to clean is It is known, such as Zhang Guiqing etc., the tungsten hydrometallurgy new cleanproduction process based on alkaline extraction technology, national rare metal Art exchanging meeting collection of thesis, the process flow disclosed in 160-171 pages, which specifically includes that under alkaline condition, uses quaternary amine Salt N263 is to containing Na2WO4And the solution of impurity P, As, Si, Mo are extracted, it is however generally that, tungsten and molybdenum are extracted into organic phase, use Water washs organic phase, and Na2CO3And P, As, Si will enter raffinate, raffinate passes through together with the washing water of organic phase It returns to tungsten oxide after causticization processing to leach, to Na therein2CO3It is recycled, and the washed rear use of the organic phase for loading tungsten NH4HCO3It is stripped, makes tungsten with (NH4)2WO4Form enters strip liquor, then after except molybdenum, evaporative crystallization obtains APT (para-tungstic acid Ammonium), NH is generated at the same time3And CO2, absorbed through water and add NH4HCO3And necessary CO2It is used as stripping agent afterwards, after back extraction Organic phase is R4NHCO3Type, through regenerating, i.e., plus NaOH control PH is allowed to be converted into (R4N)2CO3Type returns again to extraction, therefore, has Machine phase, NH3、CO2、Na2CO3It can recycle.
However, there is very strong polarity using the extracted species that N263 has extracted tungsten, in nonpolar diluent (such as 260 Number solvent naphtha) in solubility it is small, will lead to organic phase and be divided into two layers, lighter organic phase is diluent, wherein containing a small amount of extraction Close object；Heavier mainly extracted species, wherein this phenomenon is frequently referred to generate third phase containing a small amount of diluent.In practical life During production, three-phase flocculate can be generated between organic phase and raffinate, three-phase flocculate is one kind by solid, organic phase and water The mixture of phase composition, outer likeness in form jellied bean curd, and it is condensed into bulk with the increase of amount, it is suspended between two-phase interface, generates The main reason for three-phase flocculate is to contain suspended matter (silica gel, micro- mud, Ca (OH) in leachate2) and extractant be oxidized drop Solution.In extraction process, generate three-phase flocculate be usually inevitable, only measure number, but when three-phase flocculate When object is largely agglomerated and removed not in time, then it can hinder to extract split-phase, reduce WO3Transmission capacity increases organic phase consumption, when serious It will affect being normally carried out for extraction operation, or even bringing on a disaster property consequence.
For three-phase flocculate, currently used processing method mainly has addition activated clay paddling process, centrifugal process, sheet frame Filter press technique etc., but there is certain defect in these methods, for example, plus activated clay paddling process is to be added to live in three-phase flocculate Property clay stirring clarify again, float on after organic phase split-phase above recycled, the disadvantage is that large labor intensity, organic phase loss It is more, found in practical alkaline extraction and last handling process, adopt this method completely it is infeasible, and cannot achieve material return It receives, it may be possible to because three-phase flocculate is more viscous after activated clay is added, stand organic phase also not split-phase for a long time；Centrifugal process It is that three-phase flocculate is centrifuged by horizontal screw machine, it is also infeasible in actual production, the reason is that three-phase flocculate occupies It between water phase and organic phase, is separated with centrifuge, solid phase is not sunk to the bottom, and water phase and organic phase can arrange together solid phase when being discharged Out, it is difficult to separate activated clay is added；When being handled using plate compression method, due to the viscosity of three-phase flocculate Greatly, directly filtering three-phase flocculate can block filter cloth, need to frequently clear up filter cloth and filter residue is in soup shape, and the organic phase rate of recovery is low, Labor intensity of workers is big, and production efficiency is low.
Summary of the invention
Against the above technical problems, the processing method of the three-phase flocculate generated to tungsten alkaline extraction is needed to improve, While optimization processing technique, it is desirable to recycle valuable metal tungsten therein and organic phase.
Inventors have found that lime is stirred with the three-phase flocculate that tungsten alkaline extraction generates, mix, is heated, it can Three-phase flocculate is set to be demulsified, the viscosity of three-phase flocculate reduces, organic phase and solid phase, aqueous phase separation, and then is convenient for solid The subsequent processings such as liquid separation, have low in cost, simple process, additionally it is possible to tungsten therein and organic phase recycled, thus Complete the present invention.
Therefore, the method that the three-phase flocculate generated present invention firstly provides a kind of pair of tungsten alkaline extraction is handled, The described method includes: stirred tank is added in three-phase flocculate and raffinate in equal volume, stirring is opened, is added with 1 cube of total volume Lime is added in the amount of 30~50 kilograms of lime, is heated to 60-80 DEG C of stirring 1.5-3 hours, be pumped into reactive tank heat preservation 4 hours with On, filters pressing is carried out, filter residue is added roasting material as additive after diaphragm pressing and is sintered recycling tungsten therein, filtrate stream Enter separating tank, water phase is returned to production line by stratification, and organic phase returns to extraction line.
Preferably, correspond to 1 cube of three-phase flocculate and 40 kilograms of lime are added in raffinate total volume.
Preferably, after lime being added, 70 DEG C is heated to and is stirred 2 hours.
Preferably, the alkaline extraction is the extraction using N263.
Preferably, during alkaline extraction, after the three-phase flocculate runs up to 50cm, to three-phase flocculate into Row processing.
Preferably, the lime can be causticization slag.
The present invention has the advantage that
The present invention is used as inorganic agent using cheap lime (causticization slag), and success is real after mixing, stirring, heating It is now demulsified to the three-phase flocculate during tungsten alkaline extraction, so that three-phase flocculate is no longer sticky, can be led to easily It crosses filter press to be separated by solid-liquid separation, the filter residue after diaphragm pressing is aqueous, oil mass is low, and only 10-20% (uses weight-loss method pair Moisture content is measured), the tungstic acid content in filter residue merely add 0.1-0.2% (untreated three-phase flocculate it is severe In slugging, WO3Content is about 0.52%, after being handled using this method three-phase flocculate, WO in the filter residue of acquisition3Content About 0.64%), most tungsten stays in organic phase, and using colorimetrically analysing, tungstic acid content is 30- in organic phase 40g/L, and organic phase does not need activated clay regeneration, organic phase split-phase time of recycling, saturated capacity and newly matches organic phase Almost indistinction can directly return to extraction line and use, and the water phase after separation can return to production line, and filter residue can be used as additive Roasting material is added to be sintered, tungsten therein is recycled.
Specific embodiment
It will be appreciated by persons skilled in the art that the three-phase flocculate according to the present invention generated to tungsten alkaline extraction The method handled is suitable for industrial production, and the demulsification of three-phase flocculate can be arrived by direct visual perception, Also, to alkaline extraction technique, the content content of three-phase flocculate, the content of raffinate, the purity of lime, ingredient proportion etc. Harsh requirement is had no, in other words, as long as realizing the demulsification of three-phase flocculate after mixing, stirring, heating by addition lime To make it is subsequent easily material can be recycled, should all fall within the scope of protection of the present invention.
In order to more clearly be illustrated to technical solution of the present invention, make explained below:
The tungsten alkaline extraction refers to that under alkaline condition, to the technique that tungsten ore leachate is extracted, the technique is at this Field is known.Preferably, tungsten ore leachate is extracted using N263.
Extraction phase in the present invention refers to the organic of N263, diluent for containing extracted species (including tungsten and molybdenum etc.) etc. Phase, without limitation, about tens gram per liters of W content in the extraction phase.
The raffinate refers to the water phase obtained in tungsten alkaline extraction, contains P, As, Si impurity and Na in water phase2CO3、 Remaining tungsten in part etc., without limitation, Na in the raffinate2CO3Content about 60-70g/L.
Invention is further explained combined with specific embodiments below.
Prepare embodiment
On extraction line, under alkaline condition, organic be added to comprising quaternary amine N263 and No. 260 solvent naphthas is filled into tungsten In the transparent extraction tank of mine causticity leachate, stratification after heated heat preservation, separating and extracting phase (organic phase part) and raffinate Liquid (aqueous portion), while the three-phase flocculate between two-phase is observed, reach 50cm when three-phase flocculate gradually thickens When, seriously affect extraction split-phase time, WO3Exchange becomes difficult, and takes three-phase flocculate using mobile pumping.Specifically, it will pump One end pour into water, be inserted into three-phase flocculate, open pump, three-phase flocculate is pumped into metal bucket, concentrated after 50-100 barrels of collection Processing.In addition, being collected to raffinate, the processing for three-phase flocculate.
Embodiment 1
Three-phase flocculate is poured into stirred tank, is pumped into raffinate, three-phase flocculate, raffinate respectively account for totally 25 cubes of half, It opens stirring and 1 ton of lime is added, heated using steam, stirred 2 hours after being warming up to 70 DEG C, be pumped into reactive tank and keep the temperature 4 hours, open It opens filter pressing pump and carries out filters pressing, can be separated by solid-liquid separation easily, for filter residue after diaphragm pressing, aqueous oil content is only 12% (being measured using weight-loss method), after measured, WO in filter residue3Content is about 0.64%, and filter residue can be used as additive and roasting is added Imitation frosted glass is sintered, and is recycled to tungsten therein.
Filtrate flows into separating tank, and water phase is returned to production line by stratification, and organic phase returns to extraction line, using colorimetric method It analyzes, WO in organic phase3Content is about 38g/L, and organic phase does not need activated clay regeneration, when the organic phase split-phase of recycling Between, saturated capacity and newly with organic phase almost indistinction, can directly return to extraction line and use, the water phase after separation can return to life Producing line.
Comparative example 1
Three-phase flocculate is poured into stirred tank, is pumped into raffinate, three-phase flocculate, raffinate respectively account for totally 25 cubes of half, It opens stirring and 1.2 tons of causticization slags is added, heated using steam, stirred 1 hour after being warming up to 55 DEG C, it is small to be pumped into reactive tank heat preservation 5 When, it opens filter pressing pump and carries out filters pressing, but the aqueous oil content of filter residue obtained after filtering is high, viscosity is big, and filtration time is longer, recycling Poor processing effect.
Comparative example 2
Beaker is poured by 1 liter of three-phase flocculate, 100 grams of lime are added, is stirred, discovery three-phase flocculate obviously has demulsification existing As, it is placed in water-bath, is heated up to 70 degree, mobility is more preferable, stands one hour, has one layer of oil mutually to float on surface, and solid phase is in floccule, Glass bar is stained with decorating film can be washed away easily with water, be filtered with laboratory vacuum pumping filter, and organic phase and water phase can be with Solid phase separation, ratio is organic phase: water phase: solid phase is 2:1:7 (volume ratio), and oil-containing is aqueous more in the solid phase after filters pressing, face Color is in grey black, and filtration time is longer.
Comparative example 3
Beaker is poured by 1 liter of three-phase flocculate, 100 grams of activated clays are added, is stirred, three-phase flocculate is more sticky, sets In water-bath, 70 degree are heated up to, continues to stir, no significant change, glass bar, which is stained with decorating film water, to be washed away, and be sticked to glass bar On be difficult to remove, stand one day, oil-free phase is precipitated, and can not separate liquid phase and solid phase at all with laboratory vacuum pumping filter.
Above only describes better embodiments of the invention, but the present invention is not limited to above-described embodiments.This field skill Art personnel should all fall into the present invention it is understood that can be realized any same or similar means of the technology of the present invention effect Protection scope in.

Claims (6)

1. the method that the three-phase flocculate that a kind of pair of tungsten alkaline extraction generates is handled, which comprises three-phase flocculates Stirred tank is added in object and raffinate in equal volume, opens stirring, and stone is added with the amount that 30~50 kilograms of lime are added in 1 cube of total volume Ash is heated to 60-80 DEG C of stirring 1.5-3 hours, is pumped into reactive tank heat preservation 4 hours or more, carries out filters pressing, filter residue passes through diaphragm pressure Roasting material is added as additive after squeezing and is sintered recycling tungsten therein, filtrate flows into separating tank, and stratification returns water phase Retrogradation producing line, organic phase return to extraction line.
2. the method as described in claim 1, which is characterized in that add corresponding to 1 cube of three-phase flocculate with raffinate total volume Enter 40 kilograms of lime.
3. the method as described in claim 1, which is characterized in that after lime is added, is heated to 70 DEG C and stirs 2 hours.
4. the method as described in claim 1, which is characterized in that the alkaline extraction is the extraction using N263.
5. the method as described in claim 1, which is characterized in that during alkaline extraction, when the three-phase flocculate accumulates To after 50cm, three-phase flocculate is handled.
6. the method as described in claim 1, which is characterized in that the lime is causticization slag.
CN201811262449.XA 2018-10-27 2018-10-27 Treatment method of quaternary ammonium salt alkaline extraction three-phase flocculate in metal tungsten hydrometallurgy Active CN109306403B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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
CN114672648A (en) * 2022-03-07 2022-06-28 信丰华锐钨钼新材料有限公司 Method for treating N263 alkaline extraction raffinate

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2903422A1 (en) * 2006-07-03 2008-01-11 Curlook Entpr Inc METAL RECOVERY SYSTEM SUCH AS IT APPLIES TO THE LEACHING UNDER HIGH PRESSURE OF LIMONITE LATERITE ORES CONTAINING NICKEL
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
CN101935756A (en) * 2010-09-03 2011-01-05 江西明达功能材料有限责任公司 Method for reclaiming rare-earth and organic phase from third phase of rare-earth extraction
CN102876906A (en) * 2012-09-20 2013-01-16 中南大学 Method for extraction and separation of tungsten and molybdenum from tungsten and molybdenum mixed solution

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2903422A1 (en) * 2006-07-03 2008-01-11 Curlook Entpr Inc METAL RECOVERY SYSTEM SUCH AS IT APPLIES TO THE LEACHING UNDER HIGH PRESSURE OF LIMONITE LATERITE ORES CONTAINING NICKEL
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
CN101935756A (en) * 2010-09-03 2011-01-05 江西明达功能材料有限责任公司 Method for reclaiming rare-earth and organic phase from third phase of rare-earth extraction
CN102876906A (en) * 2012-09-20 2013-01-16 中南大学 Method for extraction and separation of tungsten and molybdenum from tungsten and molybdenum mixed solution

Cited By (3)

* Cited by examiner, † Cited by third party
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
CN114672648A (en) * 2022-03-07 2022-06-28 信丰华锐钨钼新材料有限公司 Method for treating N263 alkaline extraction raffinate
CN114672648B (en) * 2022-03-07 2024-06-11 赣南科技学院 Treatment method of N263 alkaline extraction raffinate

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