CN109022831A - A kind of method of amine organic phase containing molybdenum back extraction - Google Patents
A kind of method of amine organic phase containing molybdenum back extraction Download PDFInfo
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- CN109022831A CN109022831A CN201810965973.7A CN201810965973A CN109022831A CN 109022831 A CN109022831 A CN 109022831A CN 201810965973 A CN201810965973 A CN 201810965973A CN 109022831 A CN109022831 A CN 109022831A
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- organic phase
- back extraction
- containing molybdenum
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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
- C22B34/34—Obtaining molybdenum
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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
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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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- Environmental & Geological Engineering (AREA)
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Abstract
The present invention relates to a kind of methods of amine organic phase containing molybdenum back extraction, this method is stripped using single-stage or multi-stage countercurrent back extraction, in the amine organic phase containing molybdenum, the concentration of amine is 1%-20%, the concentration of molybdenum is 1g/L-30g/L, remaining group is divided into phase modifying agent and diluent, comprising the following steps: step 1, strippant is prepared, the strippant is the mixed solution of ammonium hydroxide and hydrogen peroxide；Ammonia concn range is 5%-28%；Hydrogen peroxide additional amount is the 1%-15% of ammonium hydroxide additional amount, and hydrogen peroxide concentration range is 10%-50%；Step 2 mixes back extraction with amine organic phase containing molybdenum using the prepared strippant of step 1；The stream of organic phase and water phase compares for 2:1-50:1；Stripping times are 1-10min；Being stripped temperature is 10-40 DEG C；Contact of the organic phase with water phase is comparably 4:1-1:4；The resulting mixed phase of step 2 is separated, obtains anti-stripping agent containing molybdenum and lean organic phase by step 3.The interphase impurity generated during being stripped amine organic phase containing molybdenum using method of the present invention reduces by 50% or more.
Description
Technical field
The present invention relates to solvent extractions in hydrometallurgy to extract molybdenum field, and in particular to a kind of amine is organic opposite containing molybdenum
The method of extraction.
Background technique
Existing amine extracted method, which prepares ammonium molybdate technique, to be obtained through countercurrent reextraction to back extraction using ammonium hydroxide as strippant
Take liquid and lean organic phase.The purified removal of impurities of anti-stripping agent, sulfuric acid are neutralized to after pH is 2 or so, ammonium molybdate crystal are precipitated, crystal is
For ammonium molybdate product.
There are some problems during existing molybdenum back extraction, and subproblem is in a kind of patent " back extraction of the organic phase containing molybdenum
Take method " be already mentioned above in (CN106591603A) and understood certainly, in actual back extraction operating process there is also
The problem of interphase impurity.Interphase impurity is formed between water phase and organic phase interface one layer during liquid-liquid extraction or back extraction
Solid-liquid milk.There are many reason of formation, it may be possible to: (1) in system there are suspended particulate；(2) there are colloid grains in system
Son；(3) catabolite of organic phase production；(4) the insoluble complex that catabolite and metal ion are formed.Its formation is not
It only will cause the loss of organic phase and the loss of material, but also the normal operation of equipment can be destroyed.
This patent is stripped process only for the ammonium hydroxide in amine organic phase containing molybdenum.The formation mechenism of interphase impurity is complicated,
The condition of formation is multifarious.On the one hand interphase impurity is different between different systems, on the other hand, the extraction of same system
Interphase impurity between journey and back extraction process is different, in addition, even if same back extraction process, different back extraction reagents and behaviour
Make condition, the interphase impurity formed also can be different.The method that reduces or eliminates of existing interphase impurity is not suitable for reducing
The interphase impurity generated during the back extraction of amine organic phase containing molybdenum.In the patent of publication No. CN103305693A, one is proposed
The method of kind of prevention vanadium-chromium extraction separation process interphase impurity, before this method mainly extracts depth removal by phosphorus in extraction liquid, silicon,
The impurity such as calcium, iron are extracted using the mixed solution of high efficiency composition amine extractant, demulsifier and diluent, are adjusted by extraction liquid pH
Value, control extraction temperature, time, extractant concentration and demulsifier concentration.In the patent of publication No. CN106811599A, propose
A kind of technique that control wet process metallurgy of copper leachate interphase impurity is formed, by measuring the interfacial tension of leachate, addition clay
Precipitating, when control interface tension is greater than 12.66mN/m, into subsequent back extraction and electrolytic deposition process.
Existing interphase impurity reduces or eliminates technology, for specific system effectively.And contain molybdenum for amine
The interphase impurity generated during organic phase back extraction, a kind of amine organic phase containing molybdenum that the method that there is no reduction has been the invention
The method of back extraction.
Summary of the invention
It is an object of the invention to: a kind of method of amine organic phase containing molybdenum back extraction is provided, the process of back extraction is reduced
In interphase impurity yield.
Technical scheme is as follows: a kind of method of amine organic phase containing molybdenum back extraction, this method are anti-using single-stage
Extraction or multi-stage countercurrent are stripped, and in the amine organic phase containing molybdenum, the concentration of amine is 1%-20%, and the concentration of molybdenum is 1g/L-
30g/L, remaining group are divided into phase modifying agent and diluent, comprising the following steps:
Step 1, prepares strippant, and the strippant is the mixed solution of ammonium hydroxide and hydrogen peroxide；Ammonia concn model
It encloses for 5%-28%；Hydrogen peroxide additional amount is the 1%-15% of ammonium hydroxide additional amount, and hydrogen peroxide concentration range is 10%-50%；
Step 2 mixes back extraction with amine organic phase containing molybdenum using the prepared strippant of step 1；Organic phase
Compare with the stream of water phase for 2:1-50:1；Stripping times are 1-10min；Being stripped temperature is 10-40 DEG C；Contact of the organic phase with water phase
It is comparably 4:1-1:4；
The resulting mixed phase of step 2 is separated, obtains anti-stripping agent containing molybdenum and lean organic phase by step 3.
Remarkable result of the invention is:
(1) amine organic phase containing molybdenum can be stripped using the method for amine organic phase containing molybdenum of the present invention back extraction
The interphase impurity generated during taking reduces by 50% or more；
(2) in this way, the rate of recovery of molybdenum during back extraction can be improved 2 percentage points；
(3) in this way, the organic reagent consuming cost during back extraction can be reduced；
(4) this method is used, the operability of molybdenum back extraction can be improved；The reduction of interphase impurity content is conducive to be stripped
Take going on smoothly for process；
(5) method of the invention has the advantages that process is simple, efficient, economical, environmentally friendly, practical.
Specific embodiment
Make below by method of the specific embodiment to a kind of amine organic phase containing molybdenum back extraction of the present invention into one
Step is described in detail.
The present invention can be the principle of high price molybdenum by hydrogen peroxide oxidation using low price molybdenum, by being added during back extraction
The method of hydrogen peroxide, eliminate generated during back extraction low price molybdenum precipitating, and then eliminate back extraction during due to low
Valence molybdenum precipitates the interphase impurity to be formed.
A kind of method of amine organic phase containing molybdenum back extraction, this method is stripped using single-stage or multi-stage countercurrent back extraction,
In the amine organic phase containing molybdenum, the concentration of amine is 1%-20%, and the concentration of molybdenum is 1g/L-30g/L, remaining group, which is divided into, mutually to be improved
Agent and diluent, comprising the following steps:
Step 1, prepares strippant, and the strippant is the mixed solution of ammonium hydroxide and hydrogen peroxide；
Step 2 mixes back extraction with amine organic phase containing molybdenum using the prepared strippant of step 1；
The resulting mixed phase of step 2 is separated, obtains anti-stripping agent containing molybdenum and lean organic phase by step 3.
Preferably, in strippant described in step 1, ammonia concn range is 5%-28%.
Preferably, in strippant described in step 1, hydrogen peroxide additional amount is the 1%-15% of ammonium hydroxide additional amount, dioxygen
Water concentration range is 10%-50%.
Preferably, in back extraction described in step 2, the stream of organic phase and water phase compares for 2:1-50:1.
Preferably, in back extraction described in step 2, Stripping times 1-10min.
Preferably, in back extraction described in step 2, back extraction temperature is 10-40 DEG C.
Preferably, in back extraction described in step 2, contact of the organic phase with water phase is comparably 4:1-1:4.
Embodiment
Example one:
In certain amine organic phase containing molybdenum, amine concentration 1%, molybdenum concentration 1g/L.
Using 5% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 1% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 50:1 and is comparably 4:1, incorporation time 1min, back extraction temperature is 10 DEG C.
Molybdenum concentration is 0.04g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 102g/L, and interphase impurity produces
Raw amount reduces by 55.3%.
Example two:
In certain amine organic phase containing molybdenum, amine concentration 5%, molybdenum concentration 7g/L.
Using 15% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 2% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 15:1 and is comparably 1:1, incorporation time 6min, back extraction temperature is 25 DEG C.
Molybdenum concentration is 0.06g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 106g/L, and interphase impurity produces
Raw amount reduces by 57.2%.
Example three:
In certain amine organic phase containing molybdenum, amine concentration 7.5%, molybdenum concentration 11g/L.
Using 16% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 4% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 10:1 and is comparably 1:2, incorporation time 5min, back extraction temperature is 20 DEG C.
Molybdenum concentration is 0.05g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 110g/L, and interphase impurity produces
Raw amount reduces by 56.5%.
Example four:
In certain amine organic phase containing molybdenum, amine concentration 10%, molybdenum concentration 15g/L.
Using 17% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 6% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 7:1 and is comparably 1:3, incorporation time 5min, back extraction temperature is 25 DEG C.
Molybdenum concentration is 0.04g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 103g/L, and interphase impurity produces
Raw amount reduces by 55.5%.
Example five:
In certain amine organic phase containing molybdenum, amine concentration 15%, molybdenum concentration 22g/L.
Using 18% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 8% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 5:1 and is comparably 1:1, incorporation time 5min, back extraction temperature is 20 DEG C.
Molybdenum concentration is 0.07g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 106g/L, and interphase impurity produces
Raw amount reduces by 54.7%.
Example six:
In certain amine organic phase containing molybdenum, amine concentration 20%, molybdenum concentration 30g/L.
Using 28% ammonium hydroxide as strippant, the additional amount of hydrogen peroxide is the 15% of ammonium hydroxide additional amount.
Control back extraction stream is mixed than being 2:1 and is comparably 1:4, incorporation time 10min, back extraction temperature is 40 DEG C.
Molybdenum concentration is 0.08g/L in back extraction gained lean organic phase, and anti-stripping agent molybdenum concentration is 113g/L, and interphase impurity produces
Raw amount reduces by 53.8%.
Claims (7)
1. a kind of method of amine organic phase containing molybdenum back extraction, this method is stripped using single-stage or multi-stage countercurrent back extraction, institute
It states in amine organic phase containing molybdenum, the concentration of amine is 1%-20%, and the concentration of molybdenum is 1g/L-30g/L, remaining group is divided into phase modifying agent
And diluent, which comprises the following steps:
Step 1, prepares strippant, and the strippant is the mixed solution of ammonium hydroxide and hydrogen peroxide；
Step 2 mixes back extraction with amine organic phase containing molybdenum using the prepared strippant of step 1；
The resulting mixed phase of step 2 is separated, obtains anti-stripping agent containing molybdenum and lean organic phase by step 3.
2. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 1
In strippant, ammonia concn range is 5%-28%.
3. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 1
In strippant, hydrogen peroxide additional amount is the 1%-15% of ammonium hydroxide additional amount, and hydrogen peroxide concentration range is 10%-50%.
4. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 2
In back extraction, the stream of organic phase and water phase compares for 2:1-50:1.
5. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 2
In back extraction, Stripping times 1-10min.
6. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 2
In back extraction, back extraction temperature is 10-40 DEG C.
7. a kind of method of amine organic phase containing molybdenum back extraction as described in claim 1, it is characterised in that: described in step 2
In back extraction, contact of the organic phase with water phase is comparably 4:1-1:4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041244A (en) * | 2019-12-20 | 2020-04-21 | 核工业北京化工冶金研究院 | Method for treating and recycling amine molybdenum-containing triphase substances |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225471A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Method for recovering molybdenum from water-washing molybdenum calcine wastewater |
| CN103352126A (en) * | 2013-07-25 | 2013-10-16 | 江西铜业股份有限公司 | Method for extracting ammonium molybdate from molybdenum contained waste liquid |
| CN103924104A (en) * | 2014-04-28 | 2014-07-16 | 北京矿冶研究总院 | Method for recovering molybdenum from molybdenum concentrate pressurized leaching solution |
| CN103981379A (en) * | 2014-06-04 | 2014-08-13 | 北京矿冶研究总院 | Clean extraction method of wulfenite |
| CN105420505A (en) * | 2015-12-30 | 2016-03-23 | 核工业北京化工冶金研究院 | Method for separating molybdenum from sulfuric acid precipitation mother liquor obtained in ammonium tetramolybdate preparation |
| CN106591603A (en) * | 2016-11-14 | 2017-04-26 | 核工业北京化工冶金研究院 | Back extraction method for molybdenum-containing organic phase |
| CN108342573A (en) * | 2018-03-29 | 2018-07-31 | 中南大学 | A method of from extraction and separation tungsten in ammonium tungstate solution containing molybdenum |
| CN108396143A (en) * | 2018-06-07 | 2018-08-14 | 江西理工大学 | A method of removing molybdenum from tungstate solution extraction |
-
2018
- 2018-08-23 CN CN201810965973.7A patent/CN109022831A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101225471A (en) * | 2007-12-17 | 2008-07-23 | 金堆城钼业股份有限公司 | Method for recovering molybdenum from water-washing molybdenum calcine wastewater |
| CN103352126A (en) * | 2013-07-25 | 2013-10-16 | 江西铜业股份有限公司 | Method for extracting ammonium molybdate from molybdenum contained waste liquid |
| CN103924104A (en) * | 2014-04-28 | 2014-07-16 | 北京矿冶研究总院 | Method for recovering molybdenum from molybdenum concentrate pressurized leaching solution |
| CN103981379A (en) * | 2014-06-04 | 2014-08-13 | 北京矿冶研究总院 | Clean extraction method of wulfenite |
| CN105420505A (en) * | 2015-12-30 | 2016-03-23 | 核工业北京化工冶金研究院 | Method for separating molybdenum from sulfuric acid precipitation mother liquor obtained in ammonium tetramolybdate preparation |
| CN106591603A (en) * | 2016-11-14 | 2017-04-26 | 核工业北京化工冶金研究院 | Back extraction method for molybdenum-containing organic phase |
| CN108342573A (en) * | 2018-03-29 | 2018-07-31 | 中南大学 | A method of from extraction and separation tungsten in ammonium tungstate solution containing molybdenum |
| CN108396143A (en) * | 2018-06-07 | 2018-08-14 | 江西理工大学 | A method of removing molybdenum from tungstate solution extraction |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041244A (en) * | 2019-12-20 | 2020-04-21 | 核工业北京化工冶金研究院 | Method for treating and recycling amine molybdenum-containing triphase substances |
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Application publication date: 20181218 |