CN108220629A - For the method for the extraction and separation tungsten from tungstenic aqueous solution double-aqueous phase system - Google Patents
For the method for the extraction and separation tungsten from tungstenic aqueous solution double-aqueous phase system Download PDFInfo
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- CN108220629A CN108220629A CN201810100158.4A CN201810100158A CN108220629A CN 108220629 A CN108220629 A CN 108220629A CN 201810100158 A CN201810100158 A CN 201810100158A CN 108220629 A CN108220629 A CN 108220629A
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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
- 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
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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
Abstract
A kind of method for the extraction and separation tungsten from tungstenic aqueous solution double-aqueous phase system, mainly TWEEN Series nonionic surfactant, tungstenic aqueous solution, saline solution and deionized water are mixed evenly for it, the mass fraction of nonionic surfactant is 10~20%, the mass fraction of tungsten is 0.1~5%, and the mass fraction of salt is 6~12%；PH value is adjusted to 2~3, by it after 30~60 DEG C are stirred 10~60min, is stood split-phase, be separated 10~60min of time, and it is to load the nonionic surfactant phase of tungsten to obtain phase, and lower phase is the aqueous two-phase system of water phase；40~70 DEG C, 20~60min of time of temperature is stripped, be separated 20~60min of time, and load the nonionic surfactant phase of tungsten and ammonium carbonate solution phase is comparably 1~4:1, back extraction product is ammonium tungstate.Extraction rate of the present invention is fast, phase separation is good, and tungsten (VI) single-stage extraction rate is up to more than 97%, and tungsten (VI) single-stage stripping rate is up to more than 96%.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of extracting process of tungsten.
Background technology
Tungsten is known as a kind of strategy metal, has very excellent physical and chemical performance, therefore tungsten is widely used in
The every field such as defence and military, mechanical processing, electronics industry.Tungsten industry be China strong industry, China Tungsten resource reserve, yield
It ranks first in the world with export volume.
On Tungsten smelting process aspect, most widely used now is to include soda pressuring cooking technique and sodium hydroxide decomposition work
Alkali process including skill is mainly then based on sodium hydroxide decomposition technique in China.Tungsten mineral passes through these process
Afterwards, the tungstenic solution of gained is all in alkalinity or alkalescent, can contain in usual feed liquid P, As, Si and Mo etc. must depth remove
The impurity gone.Because tungsten and molybdenum belong to same subgroup, and due to " lanthanide contract " so that the chemical property of tungsten and molybdenum is very much like, difficult
To detach, thus it is the most difficult with the separation of Mo in the impurity of tungstenic solution.The rapid development of science and technology is to a variety of materials
Harsher requirement is proposed, the material of various different performances is also constantly developed, due to unique possessed by tungsten
Performance, it is believed that its application will be more and more extensive, and various new functions also can constantly developed.Tungsten is non-renewable
Resource always has exhausted one day, so we should more treasure, and should gain more insight into it, more extensively
It studies generally, tungsten is made to play the effect of bigger in modern society.With high-quality tungsten resource exploitation totally, industrially make at present
Tungsten resource is gradually changed into complicated scheelite by wolframite.Scheelite is usually associated with largely in a manner of isomorphous
Scheelite accounts for more than the 45% of the industrial gross reserves in the tungsten resource whole nation in the high tungsten resource of China, this means that national nearly half
Tungsten ore by the output in the form of high tungsten concentrate.Therefore, the tungsten separation problem that China Tungsten smelting industry faces is very prominent.It is positive because
There is fairly obvious importance for tungsten separation, the improvement of tungsten tungsten separating technology for many years is constantly subjected to the height of metallargist
Degree is paid attention to.
Application No. is the methods that the patent of 2016110946451d proposes tungsten (VI) in a kind of extraction and separation aqueous solution, should
Method is using copolymer type surfactants, including polyoxyethylene polyoxypropylene block type polyether series (EO/PO, letter
Claim EP), polyoxyethylene polyoxypropylene polyoxyethylene blocks type polyether series (EO/PO/EO, abbreviation EPE), polyoxypropylene polyoxy second
Alkene oxypropylene block type polyether series (PO/EO/PO, abbreviation PEP) etc. form temperature-induced double-aqueous phase system with sulfate,
Tungsten in extraction and separation aqueous solution.But its pollution to environment there is also some problems, the effect of extraction is also treated further to carry
It is high.
Invention content
The purpose of the present invention is to provide one kind is simple for process, operating condition is mild, extraction efficiency is high, without using danger
The method for the extraction and separation tungsten from tungstenic aqueous solution double-aqueous phase system of the organic solvent of evil ecological environment.It is of the invention main
It is the temperature-induced double-aqueous phase system extraction and separation water being made up of TWEEN Series nonionic surfactant-sulfate-water
Tungsten in solution.
The method of the present invention includes the following steps：
(1) preparation of double-aqueous phase system solution：By nonionic surfactant, tungstenic aqueous solution, saline solution and go from
Sub- water is mixed evenly, and obtains mixed solution 1；The pH value that mixed solution 1 is adjusted with sulfuric acid, hydrochloric acid or nitric acid is 2~3, is obtained
To mixed solution 2；
In the mixed solution 1, the mass fraction of nonionic surfactant is 10~20%, and the mass fraction of tungsten is
0.1~5%, the mass fraction of salt is 6~12%；The nonionic surfactant is：TWEEN Series including Tween 80, are spat
Temperature 60, polysorbate40, polysorbas20；The source of the tungstenic aqueous solution is various tungstenic aqueous solutions；The salt includes but not limited to sulphur
Sour lithium, sodium sulphate, ammonium sulfate or magnesium sulfate.
(2) it extracts：Mixed solution 2 in step (1) is stirred at 30~60 DEG C with constant temperature blender with magnetic force, during stirring
Between for 10~60min, then it in 30~60 DEG C of thermostat water bath is stood into 10~60min of split-phase, obtains phase to load
The nonionic surfactant phase of tungsten, lower phase are the aqueous two-phase system of water phase.
(3) it is stripped：Ammonium carbonate solution is added in into the nonionic surfactant phase solution of the load tungsten of step (2),
It is 1~4 to make the nonionic surfactant phase (O) of the load tungsten value compared with water phase (A):1, the pH value of solution is adjusted with ammonium hydroxide
To 8~10, mixed solution 3 is obtained, ammonium carbonate a concentration of 20~40% in mixed solution 3, back extraction temperature is 40~70 DEG C, instead
Extraction time is 20~60min, and the phase separation time is 20~60min, and back extraction product is ammonium tungstate.
The present invention has the following advantages that compared with prior art：
1st, extraction rate is fast, good phase separation, does not form third phase and without emulsification problem, extracts tungsten (VI) concentration model
Enclose width；
2nd, single-stage extraction extraction efficiency is high, and tungsten (VI) single-stage extraction rate reaches more than 97%, tungsten (VI) single-stage stripping rate
Reach more than 96%；
3rd, it is simple for process, operating condition is mild；
4th, it is environmentally protective, it is nontoxic to environment.
Specific embodiment
Embodiment 1
(1) non-ionic surfactant Tween 80, tungstenic aqueous solution, aqueous sodium persulfate solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 80 mass fraction of non-ionic surfactant Tween is 10% in mixed solution 1, tungsten mass fraction
It is 0.1%, sodium sulfate quality score is 10%, and the pH value of mixed solution 1 is adjusted to 2 to get to mixed solution 2 with sulfuric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 30 DEG C, during stirring
Between for 60min, placed it in 30 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 20min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 2 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 8, ammonium carbonate a concentration of 20% in mixed solution 3, back extraction temperature is 40 DEG C, during back extraction
Between for 30min, the phase separation time is 50min.
After treatment, the extraction yield of tungsten (VI) is more than 97.47%, and the stripping rate of tungsten (VI) is more than 96.36%.
Embodiment 2
(1) non-ionic surfactant Tween 60, tungstenic aqueous solution, lithium sulfate aqueous solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 60 mass fraction of non-ionic surfactant Tween is 15% in mixed solution 1, tungsten mass fraction
It is 5.0%, lithium sulfate mass fraction is 8%, and the pH value of mixed solution 1 is adjusted to 2 to get to mixed solution 2 with hydrochloric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 40 DEG C, during stirring
Between for 30min, placed it in 40 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 40min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 3 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 9, ammonium carbonate a concentration of 40% in mixed solution 3, back extraction temperature is 60 DEG C, during back extraction
Between for 50min, the phase separation time is 60min.
After treatment, the extraction yield of tungsten (VI) is more than 97.76%, and the stripping rate of tungsten (VI) is more than 96.69%.
Embodiment 3
(1) non-ionic surfactant Tween 40, tungstenic aqueous solution, ammonium sulfate solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 40 mass fraction of non-ionic surfactant Tween is 20% in mixed solution 1, tungsten mass fraction
It is 2.55%, ammonium sulfate mass fraction is 12%, and the pH value of mixed solution 1 is adjusted to 2 to get to mixed solution 2 with nitric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 50 DEG C, during stirring
Between for 10min, placed it in 50 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 60min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 4 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 10, ammonium carbonate a concentration of 30% in mixed solution 3, back extraction temperature is 45 DEG C, during back extraction
Between for 20min, the phase separation time is 30min.
After treatment, the extraction yield of tungsten (VI) is more than 97.18%, and the stripping rate of tungsten (VI) is more than 96.87%.
Embodiment 4
(1) non-ionic surfactant Tween 20, tungstenic aqueous solution, magnesium sulfate solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 20 mass fraction of non-ionic surfactant Tween is 12% in mixed solution 1, tungsten mass fraction
It is 2.55%, magnesium sulfate mass fraction is 6%, and the pH value of mixed solution 1 is adjusted to 3 to get to mixed solution 2 with sulfuric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 60 DEG C, during stirring
Between for 20min, placed it in 60 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 10min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 1 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 8, ammonium carbonate a concentration of 35% in mixed solution 3, back extraction temperature is 50 DEG C, during back extraction
Between for 40min, the phase separation time is 20min.
After treatment, the extraction yield of tungsten (VI) is more than 97.43%, and the stripping rate of tungsten (VI) is more than 96.72%.
Embodiment 5
(1) non-ionic surfactant Tween 80, tungstenic aqueous solution, aqueous sodium persulfate solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 80 mass fraction of non-ionic surfactant Tween is 18% in mixed solution 1, tungsten mass fraction
It is 5%, sodium sulfate quality score is 11%, and the pH value of mixed solution 1 is adjusted to 3 to get to mixed solution 2 with hydrochloric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 60 DEG C, during stirring
Between for 40min, placed it in 60 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 30min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 2 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 9, ammonium carbonate a concentration of 25% in mixed solution 3, back extraction temperature is 65 DEG C, during back extraction
Between for 45min, the phase separation time is 40min.
After treatment, the extraction yield of tungsten (VI) is more than 97.99%, and the stripping rate of tungsten (VI) is more than 96.97%.
Embodiment 6
(1) non-ionic surfactant Tween 40, tungstenic aqueous solution, lithium sulfate aqueous solution and deionized water are mixed
Uniformly, mixed solution 1 is obtained, 40 mass fraction of non-ionic surfactant Tween is 16% in mixed solution 1, tungsten mass fraction
It is 2.55%, lithium sulfate mass fraction is 12%, and the pH value of mixed solution 1 is adjusted to 3 to get to mixed solution 2 with nitric acid；
(2) mixed solution 2 of step (1) is put into constant temperature blender with magnetic force and stirred, set temperature is 45 DEG C, during stirring
Between for 50min, placed it in 45 DEG C of thermostat water baths after stir and stand split-phase, the phase separation time is 50min, is obtained
The mutually nonionic surfactant phase for load tungsten, lower phase are the aqueous two-phase system of water phase；
(3) the nonionic surfactant phase solution of load tungsten in step (2) with ammonium carbonate solution is mixed, makes load
The nonionic surfactant phase (O) of tungsten is comparably 3 with ammonium carbonate solution phase (A)：1, obtain mixed solution 3；Use ammonium hydroxide
The pH value of mixed solution 3 is adjusted as 8, ammonium carbonate a concentration of 40% in mixed solution 3, back extraction temperature is 70 DEG C, during back extraction
Between for 60min, the phase separation time is 45min.
After treatment, the extraction yield of tungsten (VI) is more than 97.15%, and the stripping rate of tungsten (VI) is more than 96.18%.
Claims (5)
- A kind of 1. method for the extraction and separation tungsten from tungstenic aqueous solution double-aqueous phase system, it is characterised in that：It includes following Step：(1) preparation of double-aqueous phase system solution：By nonionic surfactant, tungstenic aqueous solution, saline solution and deionized water It is mixed evenly, obtains mixed solution 1；The pH value that mixed solution 1 is adjusted with sulfuric acid, hydrochloric acid or nitric acid is 2~3, is mixed Close solution 2；(2) it extracts：Mixed solution 2 in step (1) is stirred at 30~60 DEG C with constant temperature blender with magnetic force, mixing time is 10~60min, then it is stood into 10~60min of split-phase in 30~60 DEG C of thermostat water bath, it is load tungsten to obtain phase Nonionic surfactant phase, lower phase are the aqueous two-phase system of water phase；(3) it is stripped：Ammonium carbonate solution is added in into the nonionic surfactant phase solution of the load tungsten of step (2), makes to bear It is 1~4 that the nonionic surfactant phase (O) of load tungsten is worth compared with water phase (A):1, the pH value of solution is adjusted to 8 with ammonium hydroxide ~10, obtain mixed solution 3, ammonium carbonate a concentration of 20~40% in mixed solution 3, back extraction temperature is 40~70 DEG C, back extraction The time is taken as 20~60min, the phase separation time is 20~60min, and back extraction product is ammonium tungstate.
- 2. the method for tungsten in double-aqueous phase system extraction and separation aqueous solution according to claim 1, it is characterised in that：It is described mixed It closes in solution 1, the mass fraction of nonionic surfactant is 10~20%, and the mass fraction of tungsten is 0.1~5%, the matter of salt It is 6~12% to measure score.
- 3. the method for tungsten in double-aqueous phase system extraction and separation aqueous solution according to claim 1, it is characterised in that：It is described non- Ionic surface active agent is serial for tween (Tween), including but not limited to Tween 80, Tween 60, Tween 40, Tween 20。
- 4. the method for tungsten in the double-aqueous phase system extraction and separation aqueous solution according to claims 1, it is characterised in that：It is described The source of tungstenic aqueous solution is various tungstenic aqueous solutions.
- 5. the method for tungsten in the double-aqueous phase system extraction and separation aqueous solution according to claims 1, it is characterised in that：It is described Salt includes but not limited to lithium sulfate, sodium sulphate, ammonium sulfate or magnesium sulfate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226634A (en) * | 2020-09-29 | 2021-01-15 | 燕山大学 | Method for extracting and separating tungsten and molybdenum in aqueous solution by using aqueous two-phase system |
| CN112899500A (en) * | 2021-01-19 | 2021-06-04 | 燕山大学 | Method for extracting and separating tungsten and molybdenum from aqueous solution |
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| 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 |
| 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 |
| CN104760998A (en) * | 2015-04-27 | 2015-07-08 | 苏州华电北辰环保技术有限公司 | Tungsten recycling method of tungsten-containing solution based on wasted SCR denitration catalyst |
| CN106756125A (en) * | 2016-12-02 | 2017-05-31 | 燕山大学 | A kind of method of tungsten in extract and separate aqueous solution |
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2018
- 2018-02-01 CN CN201810100158.4A patent/CN108220629A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN104760998A (en) * | 2015-04-27 | 2015-07-08 | 苏州华电北辰环保技术有限公司 | Tungsten recycling method of tungsten-containing solution based on wasted SCR denitration catalyst |
| CN106756125A (en) * | 2016-12-02 | 2017-05-31 | 燕山大学 | A kind of method of tungsten in extract and separate aqueous solution |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112226634A (en) * | 2020-09-29 | 2021-01-15 | 燕山大学 | Method for extracting and separating tungsten and molybdenum in aqueous solution by using aqueous two-phase system |
| CN112899500A (en) * | 2021-01-19 | 2021-06-04 | 燕山大学 | Method for extracting and separating tungsten and molybdenum from aqueous solution |
| CN112899500B (en) * | 2021-01-19 | 2022-03-11 | 燕山大学 | Method for extracting and separating tungsten and molybdenum from aqueous solution |
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Application publication date: 20180629 |