CN105087962B - The method of high efficiency extraction molybdenum and rhenium from rhenium-containing Low Grade Molybdenum Concentrates - Google Patents
The method of high efficiency extraction molybdenum and rhenium from rhenium-containing Low Grade Molybdenum Concentrates Download PDFInfo
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- CN105087962B CN105087962B CN201510570073.9A CN201510570073A CN105087962B CN 105087962 B CN105087962 B CN 105087962B CN 201510570073 A CN201510570073 A CN 201510570073A CN 105087962 B CN105087962 B CN 105087962B
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Abstract
The invention discloses a kind of method of high efficiency extraction molybdenum and rhenium in Low Grade Molybdenum Concentrates from rhenium-containing, this method be molybdenum concntrate is made using molybdenum concntrate as core, the pelletizing using molybdenum concntrate and quick lime mixed layer as shell, pelletizing is calcined using gas-solid convection heat transfer' heat-transfer by convection mode, make the core of pelletizing that oxidizing roasting occur, shell carries out lime method roasting, not only aoxidize molybdenite and brightness rhenium ore deposit, and molybdenum, rhenium, sulphur can be retained in calcining, the high efficiente callback of molybdenum and rhenium is further realized using ammonia leaching and acid leaching process；This method sulfur-fixing rate can avoid SO2 environmental pollution up to more than 96%；And on the basis of consumption of quicklime is reduced, realize that molybdenum recovery reaches more than 92%, Rhenium recovery rate and reaches more than 85%.
Description
Technical field
The present invention relates to a kind of new method of high efficiency extraction molybdenum and rhenium from Low Grade Molybdenum Concentrates, is the low-grade molybdenum essence of rhenium-containing
The utilization of ore resources provide technical support；Belong to molybdenum metallurgical technology field.
Background technology
Molybdenum and rhenium are all strategy metal resources, and molybdenum has the advantages that high intensity, high-melting-point, resistance to grinding, corrosion-resistant, extensive
Apply to the fields such as metallurgy, space flight and aviation, photoelectric material；And rhenium is a kind of rare metal granite, its superalloy aviation,
Application in aerospace industry is increasingly extensive.
Molybdenum in China yield and consumption figure occupy first place in the world, with the continuous exploitation of molybdenum ore resource, high-grade Mo resource day
Beneficial deficient, high-quality resource is far from meeting the market demand, thus the refractory ore such as poor, thin, miscellaneous is increasingly becoming the main of extraction molybdenum
Raw material.Low Grade Molybdenum Concentrates are less than the grade requirement of standard molybdenum concntrate (containing molybdenum >=45%), its impurity SiO because of molybdenum content2、CaO、
The impurity contents such as MgO, Cu, Fe are high, cause its commercial Application difficulty big.The most association of rhenium in the mineral such as molybdenum, copper, zinc, lead, and
The rhenium raw material that carries for having value is mainly molybdenite.Molybdenum and rhenium are mainly in together with isomorph preservation, comprehensive utilization molybdenum, rhenium
Resource, it is significant to the economic value of lifting Low Grade Molybdenum Concentrates.
Primary raw material of the rhenium-containing molybdenum concntrate as extraction metal molybdenum, rhenium and its Related product, typically first by molybdenite, brightness rhenium
Ore deposit is oxidized to high price molybdenum and high price rhenium, then by leaching, extracting, the process such as clean is prepared into ammonium molybdate or rehenic acid ammonium.Contain
The oxidation of rhenium molybdenum concntrate mainly has three kinds of oxidation roasting method, lime-roasting method and pressure oxidation method typical handling process, such as the institute of table 1
Show.
Pressure oxidation method is divided into three kinds of pressure leaching, pressurized acid leaching and alkaline pressure of oxygen leaching, and its principle is to utilize in solution by force
Oxidant makes lower valency molybdenum be changed into dissolution after molybdic acid or molybdate, and its metal comprehensive recovery is high, miscellaneous containing metal suitable for processing
Rhenium-containing molybdenum concntrate more than matter, but need to set oxygen station, a large amount of strong acid of addition or highly basic or strong oxidizer, and equipment is expensive, cost
It is high, it can still produce substantial amounts of three-waste pollution thing when handling low-grade ore, making it difficult to commercial introduction application.
Domestic rhenium-containing molybdenum concntrate utilization are still based on pyrogenic process at present.Oxidizing roasting method (using air oxidation) is current
Prevailing technology, there is cost is low, production efficiency is high advantage, and do not need additive, ReS2It is oxidized to Re2O7Volatilize into
Enter flue gas, the separation of molybdenum and rhenium can be achieved.But when handling low-grade rhenium-containing molybdenum concntrate, major defect is SO in tail gas2Concentration
Low, relieving haperacidity is uneconomical, easily causes environmental pollution, and roasting process easily generate difficult volatilization rhenate and can not the molten molybdic acid of ammonia
Salt, cause the comprehensive recovery of molybdenum and rhenium relatively low.Domestic and international Ye You enterprises are utilized using lime-roasting method recovery molybdenum and rhenium, this method
Ca (ReO are formed during lime-roasting4)2And CaMoO4, and adsorb SO caused by roasting process2, environmental pollution, lime roasting can be mitigated
Though burning method is simple and easy, because lime consumption amount is big, causes the content of rhenium and molybdenum more to become dilution, extend the enrichment cycle,
Cause metal recovery rate low.
The handling process of the rhenium-containing molybdenum concntrate of table 1
To sum up analysis is understood, is still lacked one kind at present and had both been avoided that roasting process SO2Pollution problem and supplies consumption are big
Problem, while and can obtains the processing method of good molybdenum and Rhenium recovery index.Therefore, for rhenium-containing Low Grade Molybdenum Concentrates, need to open
The extracting method for sending out highly efficient.
The content of the invention
The defects of existing for the handling process of the existing molybdenum concntrate of low taste containing Lay, the purpose of the present invention is to be to provide
A kind of captured sulfur result is good, and consumption of raw materials is low, and can effectively realize molybdenum and the efficient synthetical recovery of rhenium in rhenium-containing Low Grade Molybdenum Concentrates
Method.
In order to realize the present invention technical purpose, the invention provides one kind from rhenium-containing Low Grade Molybdenum Concentrates high efficiency extraction
The method of molybdenum and rhenium, this method comprise the following steps：
(1) pelletizing with core shell structure is made in rhenium-containing Low Grade Molybdenum Concentrates；The pelletizing is with the low-grade molybdenum essence of rhenium-containing
Ore deposit is core, using the mixed layer of rhenium-containing Low Grade Molybdenum Concentrates and quick lime as shell；
(2) oxidizing roasting is carried out to the pelletizing by gas-solid convection heat transfer' heat-transfer by convection mode；
(3) oxidizing roasting product is crushed, after grinding, is leached using ammoniacal liquor, separation of solid and liquid, obtain containing ammonium molybdate and rehenic acid
Ammonium leachate and ammonia leaching residue；
(4) ammonia leaching residue is leached using sulfuric acid, separation of solid and liquid, obtains containing molybdenum and rhenium solution and acid leaching residue.
Dexterously rhenium-containing Low Grade Molybdenum Concentrates are made with core shell structure for technical scheme, and core and shell are former
Expect different pelletizings, be calcined on this basis with reference to gas-solid convection heat transfer' heat-transfer by convection mode, rhenium-containing molybdenum concntrate pelletizing kernel is played oxidation
The effect of roasting, and outer layer plays a part of lime method roasting, this method makes oxidizing roasting method and the excellent of lime method roasting lack mutually
Mend, not only can be fully oxidized by molybdenite and brightness rhenium ore deposit, and molybdenum, rhenium and sulphur are retained in calcining, effectively avoid SO2Effusion,
Solves its problem of environmental pollution；And rhenium can reclaim in follow-up leaching process, compared to the elution recovery rhenium from flue gas, rhenium is shortened
The flow of recovery；Oxidizing roasting, MoS mainly occur for core simultaneously2Only it is converted into MoO3, the consumption of roasting process quick lime can be reduced,
And the consumption of leaching process sulfuric acid, reduce the quantum of output of wet underwater welding process byproduct.
The method of high efficiency extraction molybdenum and rhenium from rhenium-containing Low Grade Molybdenum Concentrates of the present invention also includes following preferred scheme：
In preferable scheme, nuclear diameter is the 2/3~4/5 of pelletizing diameter.Technical scheme can be by regulating and controlling core
With the thickness of shell, shared proportion is calcined to oxidizing roasting and lime method and is adjusted flexibly.In order to reach optimal roasting
Effect, realizes the fixation of sulphur and molybdenum, and nuclear diameter is preferably the 2/3~4/5 of pelletizing diameter.
In preferable scheme, the addition of quick lime adds as follows in shell：M (CaO)=(1.0~1.1) ×
[M(Sn)+M(Sw)+M(Mow)], wherein, M (CaO) is CaO mole, M (S in pelletizingn) it is the mole of sulphur, M (S in corew)
For the mole of sulphur, M (Mo in shellw) be shell in molybdenum mole.The content of quick lime will adapt in shell, content mistake
It is few, the fixed effect of sulphur and molybdenum can be caused poor, and too high levels can cause quick lime and follow-up leaching reagent consumption big,
Cost is higher.
More preferably in scheme, quick lime activity degree is in 350mL4N-HClMore than.
In preferable scheme, it is 580~650 DEG C that roasting process, which controls temperature, and air velocity is 2.0~2.5m/s.
More preferably in scheme, roasting time is 1~2h.
In preferable scheme, described oxidizing roasting product is ground to granularity and is less than 0.074mm.Appropriate granularity is advantageous to
Strengthen education effect.
In preferable scheme, ammoniacal liquor leaching condition is：Ammoniacal liquor mass percent concentration is 8%~12%, liquid-solid ratio 2:1~
4:1mL/g, 60~70 DEG C of temperature.Extraction time is preferably in 2~3h.MoO can be leached by ammoniacal liquor3In molybdenum and part high price
Rhenium.
In preferable scheme, Ore Leaching condition is：H 2 so 4 concentration is 60~80g/L, liquid-solid ratio 3:1~5:1mL/g,
Temperature is 80~90 DEG C.Extraction time is preferably in 2~4h.Pass through the sour molybdenum and rhenium further leached in ammonia leaching residue.
In preferable scheme, the mass percentage content of molybdenum is less than 45% in described rhenium-containing Low Grade Molybdenum Concentrates, rhenium
Mass percentage content is 0.02~0.1%.
In preferable scheme, part rhenium-containing Low Grade Molybdenum Concentrates are first made pelletizing, then by pelletizing product low with rhenium-containing
Position molybdenum concntrate and quick lime compound carry out secondary pelletizing together, produce the pelletizing with core shell structure.
Compared with the prior art, the advantageous effects that technical scheme is brought：Technical scheme is first
The pelletizing with special core shell structure is made in rhenium-containing Low Grade Molybdenum Concentrates, on this basis using gas-solid convection heat transfer' heat-transfer by convection mode
Calcining process, can be fully oxidized by molybdenite and brightness rhenium ore deposit, and molybdenum, rhenium, sulphur are retained in calcining, is then soaked and tied using ammonia
Ore Leaching technique is closed, can realize that the high efficiente callback of molybdenum and rhenium utilizes.Technical scheme makes existing oxidizing roasting and stone
The excellent scarce complementation of grey roasting method, there is the characteristics of environmental pollution is small, depletion of additive is low, and the comprehensive recovery of molybdenum and rhenium is high；
Roasting process sulfur-fixing rate is up to more than 96%；The rate of recovery of molybdenum is up to more than 92%, and the rate of recovery of rhenium is up to more than 85%.Compare
Oxidizing roasting method is used completely, and rhenium and sulphur can be retained in calcining by technical scheme, so as to avoid SO2It evaporate into cigarette
In gas, solves its problem of environmental pollution, while rhenium can synchronously reclaim in follow-up leaching process, be reclaimed compared to being eluted from flue gas
Rhenium, shorten the flow of Rhenium recovery.And compare and be calcined completely using lime method by MoS2Calcium molybdate and calcium sulfate are converted into, due to
Pelletizing internal layer MoS of the present invention2Only it is converted into MoO3, the consumption of roasting process quick lime can be reduced, and leaching process sulfuric acid disappears
Consumption, reduce the quantum of output of wet underwater welding process byproduct.
Embodiment
For the ease of understanding the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But protection scope of the present invention is not limited to embodiment in detail below.
Unless otherwise defined, the implication that all technical terms used hereinafter are generally understood that with those skilled in the art
It is identical.Patent term used herein is intended merely to describe the purpose of specific embodiment, is not the guarantor of the limitation present invention
Protect scope.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or
Person can pass through product made from known method.
Embodiment 1
For molybdenum grade 39.27wt%, sulfur content 29.73wt%, rhenium content 0.042% molybdenum concntrate (raw material chemistry into
Point be shown in Table 1), extraction processed to it using pelletizing-roasting-ammonia leaching-acid leaching process, by molybdenum concntrate be prepared into internal layer be molybdenum concntrate,
Outer layer is the core shell structure pelletizing of molybdenum concntrate and quick lime, and internal layer diameter accounts for the 2/3 of pelletizing diameter, and addition activity degree is
350mL4N-HClQuick lime, per 1Kg molybdenum concntrates in addition 11.3molCaO (press M (CaO)=(1.0~1.1) × [M (Sn)+M
(Sw)+M(Mow)] calculate).2h is calcined under the conditions of being 2.5m/s in 580 DEG C, air velocity by pelletizing, grinds calcining after roasting
It is less than 0.074mm to granularity.It is 12% ammoniacal liquor in liquid-solid ratio 2 to use mass percent first:1st, soaked under the conditions of temperature 70 C
Go out 2h, use mass concentration to carry out secondary leaching to ammonia leaching residue for 60g/L dilute sulfuric acid after filtering, leaching parameter is liquid-solid ratio 3:
1st, 90 DEG C of extraction temperature, extraction time 2h.By the above method, roasting process sulfur-fixing rate is up to 99.2%；The overall recovery of molybdenum reaches
95.3%, the overall recovery of rhenium is up to 90.3%.
Embodiment 2
For molybdenum grade 44.13wt%, sulfur content 33.70wt%, rhenium content 0.034% molybdenum concntrate (raw material chemistry into
Point be shown in Table 1), extraction processed to it using pelletizing-roasting-ammonia leaching-acid leaching process, by molybdenum concntrate be prepared into internal layer be molybdenum concntrate,
Outer layer is the core shell structure pelletizing of molybdenum concntrate and quick lime, and internal layer diameter accounts for the 4/5 of pelletizing diameter, and addition activity degree is
400mL4N-HClQuick lime, per 1Kg molybdenum concntrates in addition 11.4molCaO (press M (CaO)=(1.0~1.1) × [M (Sn)+M
(Sw)+M(Mow)] calculate).1h is calcined under the conditions of being 2.0m/s in 650 DEG C, air velocity by pelletizing, grinds calcining after roasting
It is less than 0.074mm to granularity.It is 8% ammoniacal liquor in liquid-solid ratio 4 to use mass percent first:1st, leached under the conditions of temperature 60 C
3h, mass concentration is used to carry out secondary leaching to ammonia leaching residue for 80g/L dilute sulfuric acid after filtering, leaching parameter is liquid-solid ratio 5:1、
80 DEG C of extraction temperature, extraction time 4h.By the above method, roasting process sulfur-fixing rate is up to 98.7%；The overall recovery of molybdenum reaches
96.7%, the overall recovery of rhenium is up to 88.6%.
The Low Grade Molybdenum Concentrates chemical composition of table 1
Claims (8)
1. the method for high efficiency extraction molybdenum and rhenium from rhenium-containing Low Grade Molybdenum Concentrates, it is characterised in that：Comprise the following steps：
(1) pelletizing with core shell structure is made in rhenium-containing Low Grade Molybdenum Concentrates；The pelletizing using rhenium-containing Low Grade Molybdenum Concentrates as
Core, using the mixed layer of rhenium-containing Low Grade Molybdenum Concentrates and quick lime as shell；Described nuclear diameter is the 2/3~4/5 of pelletizing diameter；
The addition of quick lime adds as follows in described shell：M (CaO)=(1.0~1.1) × [M (Sn)+M(Sw)+M
(Mow)], wherein, M (CaO) is CaO mole, M (S in pelletizingn) it is the mole of sulphur, M (S in corew) it is sulphur in shell
Mole, M (Mow) be shell in molybdenum mole；
(2) oxidizing roasting is carried out to the pelletizing by gas-solid convection heat transfer' heat-transfer by convection mode；
(3) oxidizing roasting product is crushed, after grinding, leached using ammoniacal liquor, separation of solid and liquid, obtain soaking containing ammonium molybdate and rehenic acid ammonium
Go out liquid and ammonia leaching residue；
(4) ammonia leaching residue is leached using sulfuric acid, separation of solid and liquid, obtains containing molybdenum and rhenium solution and acid leaching residue.
2. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
Described quick lime activity degree is in 350mL4N-HClMore than.
3. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
Described oxidizing roasting process control temp is 580~650 DEG C, and air velocity is 2.0~2.5m/s.
4. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 3 from rhenium-containing, it is characterised in that：
Oxidizing roasting time is 1~2h.
5. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
Described oxidizing roasting product, which crushes, is ground to granularity is less than 0.074mm.
6. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
Ammoniacal liquor leaching condition is：Ammoniacal liquor mass percent concentration is 8%~12%, liquid-solid ratio 2:1~4:1mL/g, 60~70 DEG C of temperature.
7. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
Ore Leaching condition is：H 2 so 4 concentration is 60~80g/L, liquid-solid ratio 3:1~5:1mL/g, temperature are 80~90 DEG C.
8. the method for high efficiency extraction molybdenum and rhenium in the Low Grade Molybdenum Concentrates according to claim 1 from rhenium-containing, it is characterised in that：
The mass percentage content of molybdenum is less than 45% in described rhenium-containing Low Grade Molybdenum Concentrates, the mass percentage content of rhenium for 0.02~
0.1%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3770414A (en) * | 1970-12-28 | 1973-11-06 | Continental Ore Corp | Recovery of rhenium and molybdenum values from molybdenite concentrates |
| CN102051483A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Method for reclaiming metals from molybdenum-containing waste catalyst |
| CN104232941A (en) * | 2014-09-11 | 2014-12-24 | 陕西炼石矿业有限公司 | Method for comprehensive recovery of molybdenum and rhenium from high molybdenum-rhenium concentrate |
-
2015
- 2015-09-09 CN CN201510570073.9A patent/CN105087962B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3770414A (en) * | 1970-12-28 | 1973-11-06 | Continental Ore Corp | Recovery of rhenium and molybdenum values from molybdenite concentrates |
| CN102051483A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Method for reclaiming metals from molybdenum-containing waste catalyst |
| CN104232941A (en) * | 2014-09-11 | 2014-12-24 | 陕西炼石矿业有限公司 | Method for comprehensive recovery of molybdenum and rhenium from high molybdenum-rhenium concentrate |
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