CN107058752A - A kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust - Google Patents
A kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust Download PDFInfo
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- CN107058752A CN107058752A CN201710154374.2A CN201710154374A CN107058752A CN 107058752 A CN107058752 A CN 107058752A CN 201710154374 A CN201710154374 A CN 201710154374A CN 107058752 A CN107058752 A CN 107058752A
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- Prior art keywords
- rhenium
- flue dust
- molybdenum
- ore concentrate
- vacuum distillation
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/02—Working-up flue dust
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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
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
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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
The invention provides a kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method adds calcining molybdenum ore concentrate flue dust in vacuum distillation furnace, vacuum furnace pressure is evacuated to for below 200Pa, begin to warm up, vapo(u)rizing temperature in vacuum distillation furnace is 200 DEG C~500 DEG C, then it is incubated, soaking time is 1~10 hour, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.The method of the present invention is to realize the separation of rhenium, molybdenum in flue dust using the rhenium oxide in flue dust and vapour pressure difference rhenium of the molybdenum oxide in different temperatures, and realizes the enrichment method of rhenium.Substantial amounts of molybdenum oxide can be separated in still-process, and rhenium oxide is enriched with distillate, and also a small part molybdenum oxide is present in distillate, is easy to the separating technology of follow-up rhenium, molybdenum.This method is easy to operate, and energy utilization rate and the efficiency of heating surface are high, and safety and sanitation are pollution-free.
Description
Technical field
The invention belongs to molybdenum industrial circle, it is related to calcining molybdenum ore concentrate flue dust, and in particular to one kind is concentrated with vacuum distillation furnace
It is enriched with the method for rhenium in calcining molybdenum ore concentrate flue dust.
Background technology
Rhenium is a kind of rare and scatter element, and without Independent Mineral, its usual association is among molybdenum ore and copper mine, in molybdenum concntrate
Content is 17-20mg/kg, and such content, which directly extracts rhenium metal, sizable difficulty, economically also uneconomical.Generally
Molybdenum concntrate is during oxidizing roasting, the ReS in concentrate2It can be oxidized to, due to Re2O7Low boiling point (360 DEG C), can be with
Flue gas enters dust collecting system, part Re2O7Can be by SO in flue gas2Etc. being reduced to Re2O3(adiabatic condensation temperature is 270 DEG C) etc., due to
Dust collecting system requires stricter to flue-gas temperature, it usually needs by flue-gas temperature control below 200 DEG C, therefore make major part
Rhenium oxide condense in the flue dust of dust collecting system, after measured, in calcining molybdenum ore concentrate flue dust rhenium content generally in 60-
Between 3000mg/kg, molybdenum content is between 40-50%.
The recovery method of rhenium mainly uses the solution such as acid or water to the rhenium in flue dust in current calcining molybdenum ore concentrate flue dust
Leached, obtain rhenium-containing, the leachate of molybdenum, to the rhenium in leachate using extraction, the isolation technics such as ion exchange by rhenium and
Molybdenum and other separation of foreign elements in leachate.These methods are both needed to problems faced：1) leaching process material handling capacity
Greatly, because the rhenium content in flue dust is relatively low, in order to obtain rhenium leachate, it is necessary to which substantial amounts of flue dust is leached；2) leachate
Middle molybdenum content is high, causes the separation of rhenium molybdenum difficult, and during leaching flue dust, not only rhenium enters solution, also has substantial amounts of molybdenum
It is still and rhenium, molybdenum two based on molybdenum because molybdenum is main component in flue dust, therefore in the leachate obtained into solution
Element property is planted close, it is necessary to which extractant has very high rhenium molybdenum separation for extract and separate；To ionic energy transfer
Speech is, it is necessary to which ion exchange resin not only has very high rhenium molybdenum separation, in addition it is also necessary to have larger exchange capacity, and full
, it is necessary to carry out rhenium, the parsing of molybdenum respectively when being parsed with resin, therefore cause that desorbed solution consumption is big, resin consumptions big, reclaim
The problems such as desorbed solution treating capacity after rhenium, molybdenum is big.
The content of the invention
Based on problems of the prior art, the present invention proposes the roasting of one kind vacuum distillation furnace enrichment method molybdenum concntrate
The method of rhenium in flue dust is burnt, the rhenium progress enrichment concentration solved in calcining molybdenum ore concentrate flue dust in the prior art is needed whole flue dust
Immersion is reclaimed, quantities it is big and obtain rhenium-containing, two kinds of materials are difficult to the technical problem separated in the leachate of molybdenum.
In order to solve the above-mentioned technical problem, the application, which is adopted the following technical scheme that, is achieved：
A kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method is by calcining molybdenum ore concentrate cigarette
Dirt is added in vacuum distillation furnace, is evacuated to vacuum furnace pressure for below 200Pa, is begun to warm up, the steaming in vacuum distillation furnace
Temperature is evaporated for 200 DEG C~500 DEG C, is then incubated, soaking time is 1~10 hour, and the distillate for collecting distillation acquisition is richness
Rhenium-containing material after collection concentration.
The present invention also has following distinguishing feature：
It is preferred that, described vapo(u)rizing temperature is 300 DEG C~500 DEG C.
It is furthermore preferred that described vapo(u)rizing temperature is 400 DEG C.
It is preferred that, described soaking time is 2~4 hours.
It is furthermore preferred that described soaking time is 3 hours.
Described calcining molybdenum ore concentrate flue dust be molybdenum concntrate obtained in roasting process rhenium-containing flue dust, molybdenum-iron smelting process receive
The rhenium-containing flue dust that the flue dust and/or rhenium-containing copper mine of collection are collected in smelting process.
Compared with prior art, beneficial has the technical effect that the present invention：
(I) method of the invention is to utilize the rhenium oxide and vapour pressure deficit of the molybdenum oxide in different temperatures in flue dust
Different rhenium realizes the separation of rhenium in flue dust, molybdenum, and realizes the enrichment method of rhenium.Substantial amounts of molybdenum oxide can be divided in still-process
Separate out, in distillate rhenium oxide be enriched with, an also small part molybdenum oxide exist in distillate, be easy to follow-up rhenium,
The separating technology of molybdenum.
This method is easy to operate, and energy utilization rate and the efficiency of heating surface are high, and safety and sanitation are pollution-free.
(II) rhenium content is high in the rich rhenium material after the enrichment concentration that method of the invention is obtained, and material total amount is small, helps
In reduce rhenium leaching process material handling capacity, while reduce leachate in molybdenum-rhenium concentration ratio, be conducive to rhenium in leachate,
The separation and Extraction of molybdenum, this method has enrichment concentration, and speed is fast, production efficiency is high, the features such as bioaccumulation efficiency of rhenium is high.
(III) during the rhenium of method of the invention in enrichment method flue dust, the chemicals of other materials will not be destroyed
Phase, short with flow, the cycle is short, efficiency high, the characteristics of comprehensive resource utilization rate is high, can greatly improve the separation of rhenium in flue dust
Efficiency.
(IV) the rhenium content in the distillate of method acquisition of the invention is used for 23.75%~32.1%, still-process
The yield of middle rhenium is 85%~95%.
The particular content of the present invention is described in more detail with reference to embodiments.
Embodiment
The principle of the present invention is that in calcining molybdenum ore concentrate flue dust, the oxide for the rhenium being relatively stabilized has Re2O7、ReO3With
ReO, according to the property of each oxide, ReO3400 DEG C are decomposed into Re in vacuum environment2O7And ReO2, ReO is in vacuum environment>
500 DEG C can be analyzed to Re2O7And Re.And the steaming of the oxide of the vapour pressure of the oxide of the molybdenum in calcining molybdenum ore concentrate flue dust and rhenium
Air pressure has larger difference, it is possible to use this property is separated the rhenium in flue dust, molybdenum, so as to realize the dense of rhenium in flue dust
Contracting enrichment.
Above-mentioned technical proposal, specific embodiment of the invention given below are deferred to, it is necessary to which explanation is the present invention not office
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
Enclose.The present invention is described in further details with reference to embodiment.
It should be noted that in following embodiments, calcining molybdenum ore concentrate flue dust is containing that molybdenum concntrate is obtained in roasting process
Rhenium flue dust.The flue dust or the rhenium-containing flue dust that be collected in smelting process of rhenium-containing copper mine that can also be collected using molybdenum-iron smelting process come
Replace.
It should be noted that in following embodiments, in the rhenium-containing material after enrichment concentration, rhenium element is with the oxide of rhenium
Form is present, and oxide is with Re2O7Based on.
Embodiment 1：
The method that the present embodiment provides rhenium in a kind of use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method
Detailed process is：The content for taking rhenium element in 0.5kg calcining molybdenum ore concentrate flue dust, flue dust is 3000mg/kg, and the content of molybdenum element is
The 45% of calcining molybdenum ore concentrate flue dust gross mass, calcining molybdenum ore concentrate flue dust is placed in graphite crucible and is put into vacuum distillation furnace, is opened
Open vavuum pump so that vacuum furnace pressure reaches below 200Pa, begins to warm up, be heated to being incubated 4 hours during 300 DEG C of temperature, protect
Temperature is cooled to vacuum breaker after normal temperature after terminating, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.
Distillate is weighed, analyzed the content of rhenium element therein, after vacuum distillation, obtain 4g distillates, with
Rhenium content in the quality meter of element, distillate is that the yield of rhenium in 31.9%, still-process is 85%.
Embodiment 2：
The method that the present embodiment provides rhenium in a kind of use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method
Detailed process is：The content for taking rhenium element in 0.5kg calcining molybdenum ore concentrate flue dust, flue dust is 3000mg/kg, and the content of molybdenum element is
The 45% of calcining molybdenum ore concentrate flue dust gross mass, calcining molybdenum ore concentrate flue dust is placed in graphite crucible and is put into vacuum distillation furnace, is opened
Open vavuum pump so that vacuum furnace pressure reaches below 200Pa, begins to warm up, be heated to being incubated 3 hours during 400 DEG C of temperature, protect
Temperature is cooled to vacuum breaker after normal temperature after terminating, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.
Distillate is weighed, analyzed the content of rhenium element therein, after vacuum distillation, obtains 4.2g distillates,
In terms of the quality of element, the rhenium content in distillate is that the yield of rhenium in 32.1%, still-process is 90%.
Embodiment 3：
The method that the present embodiment provides rhenium in a kind of use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method
Detailed process is：The content for taking rhenium element in 0.5kg calcining molybdenum ore concentrate flue dust, flue dust is 3000mg/kg, and the content of molybdenum element is
The 45% of calcining molybdenum ore concentrate flue dust gross mass, calcining molybdenum ore concentrate flue dust is placed in graphite crucible and is put into vacuum distillation furnace, is opened
Open vavuum pump so that vacuum furnace pressure reaches below 200Pa, begins to warm up, be heated to being incubated 2 hours during 500 DEG C of temperature, protect
Temperature is cooled to vacuum breaker after normal temperature after terminating, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.
Distillate is weighed, analyzed the content of rhenium element therein, after vacuum distillation, obtains 5.5g distillates,
In terms of the quality of element, the rhenium content in distillate is that the yield of rhenium in 23.75%, still-process is 95%.
Comparative example 1：
The method that this comparative example provides rhenium in a kind of use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method
Detailed process is：The content for taking rhenium element in 0.5kg calcining molybdenum ore concentrate flue dust, flue dust is 3000mg/kg, and the content of molybdenum element is
The 45% of calcining molybdenum ore concentrate flue dust gross mass, calcining molybdenum ore concentrate flue dust is placed in graphite crucible and is put into vacuum distillation furnace, is opened
Open vavuum pump so that vacuum furnace pressure reaches below 200Pa, begins to warm up, be heated to being incubated 2 hours during 600 DEG C of temperature, protect
Temperature is cooled to vacuum breaker after normal temperature after terminating, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.
Distillate is weighed, analyzed the content of rhenium element therein, after vacuum distillation, obtains 20.5g distillates,
In terms of the quality of element, the rhenium content in distillate is that the yield of rhenium in 6.95%, still-process is 95%.
Comparative example 2：
The method that this comparative example provides rhenium in a kind of use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, this method
Detailed process is：The content for taking rhenium element in 0.5kg calcining molybdenum ore concentrate flue dust, flue dust is 3000mg/kg, and the content of molybdenum element is
The 45% of calcining molybdenum ore concentrate flue dust gross mass, calcining molybdenum ore concentrate flue dust is placed in graphite crucible and is put into vacuum distillation furnace, is opened
Open vavuum pump so that vacuum furnace pressure reaches below 200Pa, begins to warm up, be heated to being incubated 10 hours during 100 DEG C of temperature,
Insulation is cooled to vacuum breaker after normal temperature after terminating, the distillate for collecting distillation acquisition is the rhenium-containing material after enrichment concentration.
Distillate is weighed, analyzed the content of rhenium element therein, after vacuum distillation, distillate is not obtained.
The increase with vapo(u)rizing temperature is can be seen that from above-described embodiment and comparative example, the rate of recovery of rhenium does not increase substantially,
But the product of distillation amount increase obtained, main reason is that, temperature is raised, MoO present in flue dust3It is distilled into distillation production
Thing, product of distillation amount increase, although the evaporation rate of recovery of rhenium is unchanged, but rhenium content is reduced in product, can increase follow-up distillation production
Rhenium, the difficulty of molybdenum separation in the processing procedure of thing；When vapo(u)rizing temperature is relatively low, Re2O7Vapour pressure it is too small, it is impossible to by Re2O7Distillation
Out, product of distillation therefore is not obtained, it is impossible to reach the purpose of distillation and concentration rhenium.
Claims (6)
1. a kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust, it is characterised in that this method is by molybdenum
Concentrate calcination fume is added in vacuum distillation furnace, is evacuated to vacuum furnace pressure for below 200Pa, is begun to warm up, vacuum is steamed
Vapo(u)rizing temperature in furnace is 200 DEG C~500 DEG C, is then incubated, and soaking time is 1~10 hour, collects evaporating for distillation acquisition
It is the rhenium-containing material after enrichment concentration to go out thing.
2. the method as described in claim 1, it is characterised in that described vapo(u)rizing temperature is 300 DEG C~500 DEG C.
3. method as claimed in claim 2, it is characterised in that described vapo(u)rizing temperature is 400 DEG C.
4. the method as described in claim 1, it is characterised in that described soaking time is 2~4 hours.
5. method as claimed in claim 4, it is characterised in that described soaking time is 3 hours.
6. the method as described in claim 1, it is characterised in that described calcining molybdenum ore concentrate flue dust is molybdenum concntrate in roasting process
The rhenium-containing cigarette that the flue dust and/or rhenium-containing copper mine that the rhenium-containing flue dust of middle acquisition, molybdenum-iron smelting process are collected are collected in smelting process
Dirt.
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Application publication date: 20170818 |