CN105219980B - A kind of method for extracting rhenium - Google Patents
A kind of method for extracting rhenium Download PDFInfo
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- CN105219980B CN105219980B CN201510720521.9A CN201510720521A CN105219980B CN 105219980 B CN105219980 B CN 105219980B CN 201510720521 A CN201510720521 A CN 201510720521A CN 105219980 B CN105219980 B CN 105219980B
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Abstract
Technical field is utilized the present invention relates to Rhenium recovery, and in particular to a kind of method of extraction rhenium.The method of the extraction rhenium of proposition, with rhenium-containing ore deposit as raw material, obtains rhenium-containing extract solution, and realize that tail gas safe is discharged by residual air process step using the oxidizing roasting of rhenium-containing ore deposit, baking flue gas high-temperature dust removal and rhenium oxide gas absorption step.The present invention is by the improvement to the furnace body that seethes with excitement and controls rational oxidizing roasting, dedusting and gas absorption technique condition, improves the oxidizing roasting efficiency and rhenium volatility of rhenium-containing ore deposit, reduces roasting Dust Capacity, improves production efficiency；Dedusting method and gas absorption system are improved, loss of the rhenium-containing flue gas in dedusting and gas absorption process is reduced；The recycled in its entirety rate that oxidizing roasting mode extracts rhenium is improved, rhenium oxidizing roasting efficiency is low in fluidized bed furnace, rhenium volatility is low when solving the problems, such as that existing regular oxidation baking modes extract rhenium, rhenium loses big in dedusting and gas absorption process.
Description
Technical field
Technical field is utilized the present invention relates to Rhenium recovery, and in particular to a kind of method of extraction rhenium, it is particularly a kind of from containing
The method that rhenium obtains rhenium-containing extract solution is extracted in the oxidizing roasting of rhenium ore deposit.
Background technology
Precious metal rhenium and its compound, due to special physics, chemical property, such as electric conductivity, catalysis activity,
At numerous aspects such as petrochemical industry platinum-rhenium reforming catalyst, the development of military project material, high-temperature material and novel environment friendly compounds
It is widely used.
Because nature is in itself without independent rhenium mineral deposit, rhenium is main and molybdenum ore or copper mine association coexist, the rhenium of existing market
Supply source, is to process the byproduct obtained in molybdenum ore or copper mine.From the point of view of the technology according to disclosed in domestic and international, rhenium product return
Receive and production mainly uses following approach：The first step is decomposed by wet method or pyrogenic process and for rhenium rhenium-containing extraction is transferred to from rhenium-containing ore deposit
In liquid；Second step enriching and recovering rhenium from rhenium-containing extract solution by solvent extraction, ion exchange or charcoal absorption etc.；3rd
Step, rhenium compound or rhenium metal are prepared from the rich further purification of Rhenium recovery liquid.
By Wet Decomposition, technical research rhenium being transferred in rhenium-containing extract solution to extract rhenium is more：The Ministry of Internal Affairs of the U.S.
（The Uniter States of America as represented by the Secretary of the Interior
, US3849265）The electronics method for oxidation of molybdenum and rhenium is reclaimed in the ore of proposition, raw material is dissolved in water-soluble salt solution and then in electricity
Electrolytic oxidation being carried out in solution groove and reclaiming molybdenum and rhenium, during concrete operations, prepare pumpable dispersions, the suspension is by sulfuration rhenium solid
Constituted with the mixture that can convey liquid, liquid is water salting liquid, will be powered between anode, keep pH of suspension in 5-9, temperature
15-55 DEG C, suspension is electrolysed, separated, obtain residual comprising soluble molybdenum, the aqueous solution of rhenium or molybdenum-rhenium mixture and electrolysis solid
Slag, then carry out molybdenum-rhenium extraction and recovery；In addition, GTE happiness Wan Nian companies（GTE Sylvania Incorporated,Seneca
Falls, N.Y., US3725524）What is proposed reclaims method, the Beckman Alexandria of molybdenum and rhenium from sulphide ore
（Beckmann, Alexander, EP0041841A1）The method that metal is reclaimed from metallic ore such as rhenium ore deposit of proposition,
MetLeach Co., Ltds（MetaLeach Limited, WO/2011/113080A）Propose from the sulphur containing molybdenum and/or rhenium
Change（Essence）The method and WRC world resources Co., Ltd of Leaching Molybdenum and rhenium in ore deposit（World Resources Company,
US20130078166）What is proposed reclaims rhenium and the method for other metals from rhenium-containing mineral, carries out in the solution.Can
To find, these Wet Decompositions are extracted in the method for rhenium, and rhenium-containing extract solution post processor is complicated, causes long flow path, rhenium entirety
Extraction recovery is low.
At home, extracted from rhenium-containing ore deposit and reclaim rhenium, most traditional is also that topmost extracting method is carried using pyrogenic process
Take, i.e. oxidizing roasting；It is as follows that principle is extracted in the oxidizing roasting of rhenium：
When rhenium-containing ore deposit is calcined under aerobic conditions, sulfuration rhenium（Including Re2S7And ReS2）It is oxidized to high price rhenium oxygen
Compound Re2O7。Re2O7Boiling point be 361 DEG C, low boiling point, high volatility is volatized into flue gas under the sintering temperature of molybdenum concntrate
In, extracting reaction is（Zhang Qixiu, Zhao Qinsheng are edited,《Tungsten is metallurgical》, in September, 2005, page 212）：2Re2S7+21O2=
2Re2O7 + 14SO2, 4ReS2+15O2=2 Re2O7 +8SO2；After flue gas removing dust, gaseous state rhenium oxide Re2O7Drenched into flue gas
Wash, Re2O7It is dissolved in water generation perrhenic acid, Re2O7+H2O= 2HReO4, rhenium-containing extract solution is obtained, it is further carried out Rhenium recovery.
Jilin Iron Alloy Plant（Application, extraction and the market analysis of rhenium, analogy celebrating China, mineral products comprehensive utilization, phase nineteen ninety-five the 3rd）
It is manufacturer that China reclaims rhenium earliest, is calcined using multiple hearth furnace, flue gas is gathered dust by dry type electricity, wet type electricity gathers dust, finally
Absorbed with water, through extraction, after be changed to ion exchange production ammonium perrhenate, the total recovery of rhenium only has 50%；The auspicious smooth copper industry of Yanggu is limited
Company（CN201210099836.2）The method for proposing extraction rhenium in a kind of rich rhenium concentrate, comprises the following steps：By rich rhenium concentrate
It is mixed and finely ground with quick lime, compound is passed through oxygen-enriched air in electric furnace and is calcined at 400 DEG C~900 DEG C, after roasting
Material water size mixing leaching, leaching is filtered after finishing, and adds cleaner to remove calcium and micro heavy ion liquid after filter, is removed
Filtered after miscellaneous, liquid after the filter after removal of impurities is filtered is carried out into ion exchange with anion exchange resin, rehenic acid is obtained after desorption
Ammonium salt solution, then condensing crystallizing obtains ammonium perrhenate.
From the point of view of the technology of above-mentioned domestic and international extraction rhenium, although wet oxidation and pyrogenic process oxidizing roasting method can be from containing
Extract rhenium in rhenium ore deposit, but wet oxidation post processing trouble and molybdenum-rhenium separate it is difficult, due to rhenium be association in molybdenum ore or copper mine, and molybdenum
Ore deposit and copper mine are mainly to be smelted using pyrogenic process method for oxidation, therefore pyrogenic process oxidation is still most traditional and topmost extraction rhenium
Means, in WRC world resources Co., Ltd（World Resources Company, US 2,013 00 78 166）Disclosed skill
It is on the basis of wet underwater welding obtains rhenium disulfide, sulfuration rhenium to be oxidized to by rhenium using oxidizing roasting method and is aoxidized in art
Thing, 2Re2S7+21O2+heat= 2Re2O7(distillation)+14SO2, rhenium oxide is entered flue gas, reprocessing flue gas obtains rhenium high
Sour ammonium.But in the existing method using pyrogenic process extraction rhenium, however it remains following problems：
First, during using rhenium-containing ore deposit, such as rhenium is extracted in molybdenum concntrate oxidizing roasting, early stage simple reverberatory furnace, at present extensively
Rotary kiln, multiple hearth furnace, because ore particle is piled up, although the artificial passage furnace charge, mechanical rake of stirring is respectively adopted and stirs passage stove
The mode that furnace charge is stirred in material or the interior flight lifting of kiln cylinder solves the problems, such as the stirring of roasting process furnace charge, but mineral are contacted with oxygen source
It is insufficient, have that oxidation sweetening efficiency is low, roasting time is long, the low problem of Rhenium recovery rate, rough Statistics, in smelting process
In, because the valuable rare element rhenium oxidation of association in molybdenite is insufficient and is lost with flue gas, Rhenium recovery rate only 70% or so；
And using the fluidization oxidizing roasting method of fluidized bed furnace, because mineral can be fully contacted with oxygen, and discharging can be fed with continous way,
Oxidizing roasting efficiency and production capacity are greatly improved, and can obtain up to 85%~97% volatility（The application of rhenium, carry
Take and market analysis, analogy celebrating China, mineral products comprehensive utilization, phase nineteen ninety-five the 3rd）；
But because the existing boiling furnace body for being conventionally used for calcining molybdenum concentrate is an isometrical cylindrical refractory chamber（（Zhang Qi
Repair, Zhao Qinsheng chief editors,《Tungsten is metallurgical》, in September, 2005, Fig. 4-7 molybdenite concentrate fluosolids roastings technological process signal of page 171
Figure）, after rhenium-containing mineral aggregate contacts mixing with oxygen source, constantly flowed up when oxidation reaction is carried out, flow through discharging in mixing pattern
Still degree is flowed up in tempo after mouthful, and the dust that flue gas is carried constantly enters follow-up dust pelletizing system by flue, causes dust
Amount is excessive, is also difficult to ensure that the oxidization time of rhenium；And when rhenium-containing ore deposit is calcined, it is ensured that the fully oxidized effusion of rhenium, boiling
Oxygen content should ensure that ReS in stove2→Re2O7Conversion ratio；
Secondly, it is general to be gathered dust using conventional bagroom during flue gas ash removal, such as Luanchuanmolybdenum group
Limited company（CN201210129459.2）The dust pelletizing system for being constituted using cyclone dust collectors and bagroom is carried out
Gather dust, with molybdenum calcining（Molybdenum oxide）To be feasible under the process conditions of target product, but due to the fibre of bagroom
Dimension heat resistance is low, and generally below 300 DEG C, flue gas need to carry out radiating and cooling in advance and gas dilution just can guarantee that bagroom
Normal work, in radiating and cooling and gas dilution, because oxidation simultaneously enter flue gas gaseous state rhenium oxide can because drop
Temperature crystallization and be mixed into the flue dust retained by bagroom, only part rhenium oxide can be operated into absorption and carries by drip washing
Take in liquid, cause rhenium to be carried out as byproduct partially recycled, the serious extraction recovery for reducing rhenium；
3rd, when the gas absorption stage rhenium is absorbed, usual manner is that have to be highly soluble in water generation using rhenium oxide
The characteristic of perrhenic acid, rhenium-containing absorbing liquid is obtained by the rhenium composition absorbed with Water spray or filler water absorption pattern in flue gas,
But in practice, even across multiple cyclic absorption, the rhenium concentration of absorption extraction liquid is also no longer improved, but it is dynamically flat to reach certain
Weighing apparatus, can only obtain the even lower extract solutions of rhenium content about 0.05g/L, and absorptivity is low；
Above-mentioned these problems, i.e., during oxidizing roasting rhenium oxidizing roasting efficiency and volatility is low, flue gas ash removal loss and
Absorb the superposition of the factor such as incomplete so that in obtaining the whole flow process of rhenium-containing extract solution from rhenium-containing ore deposit oxidizing roasting extraction rhenium,
Rhenium extraction recovery only 50~70%, has a strong impact on the recycling of rhenium, hinders the fast development of rhenium industry.
The content of the invention
It is an object of the invention to provide a kind of method for extracting rhenium, rhenium is extracted to solve existing regular oxidation baking modes
When rhenium oxidizing roasting efficiency is low in fluidized bed furnace, rhenium volatility is low, rhenium loses big problem in dedusting and gas absorption process,
The present invention is by the improvement to the furnace body that seethes with excitement and controls rational oxidizing roasting, dedusting and gas absorption technique condition, improves
The oxidizing roasting efficiency and rhenium volatility of rhenium-containing ore deposit, reduce roasting Dust Capacity, improve production efficiency；Improve dedusting side
Formula and gas absorption system, reduce loss of the rhenium-containing flue gas in dedusting and gas absorption process；Improve oxidizing roasting side
Formula extracts the recycled in its entirety rate of rhenium, can promote rhenium extraction and the fast development of rhenium application industry.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of method for extracting rhenium, comprises the technical steps that：
（1）Rhenium-containing ore deposit oxidizing roasting
Rhenium-containing ore deposit is sent into fluidized bed furnace, is contacted with oxygen-containing air and is calcined；The boiling furnace body is provided with hybrid reaction
Area and second reaction zone, the second reaction zone is higher than discharging opening and is sequentially provided with extension diameter section and undergauge section, institute upwards along body of heater
State extension diameter section and compare 1.1-1.8 with hybrid reaction area diameter：1, extension diameter section is truncated cone-shaped, its vertical profile with hybrid reaction area binding site
Face is isosceles trapezoid, and the base angle of round platform is 15~30o, and the undergauge section is with hybrid reaction area diameter than 0.3~0.5：1, undergauge
Section is truncated cone-shaped with extension diameter section binding site, and its vertical section is isosceles trapezoid, and the apex angle ss of round platform is 110~145o, the undergauge
Section outlet is connected with the exhanst gas outlet on body of heater；During oxidizing roasting, control the coefficient of excess air of oxygen-containing air for 1.2~
2.5%, 560~700 DEG C of hybrid reaction area sintering temperature, 23~180KPa of partial pressure of oxygen, the flue gas for being calcined generation carries dust through contracting
Footpath section is discharged by exhanst gas outlet；
（2）Baking flue gas high-temperature dust removal
Baking flue gas are introduced into dust pelletizing system, in dust removal process, it is 405~450 to keep flue gas temperature in dust pelletizing system
DEG C, obtained after dedusting except dust and gas and dust；
（3）Rhenium oxide gas absorbs
Gas absorption system will be introduced except dust and gas, keep gas absorption system absorption liquid pH >=4, absorbed except the rhenium in dust and gas
Oxide Re2O7With sulfur dioxide SO2, obtain rhenium-containing extract solution and residual air；
（4）Residual air treatment
Residual air after being absorbed through gas introduces residual air processing system, carries out residual air treatment regeneration, the titanium dioxide after regeneration
Sulphur returns to oxidizing roasting step, the oxidizing roasting of rhenium-containing ore deposit is used for after mixing with oxygen-containing air, or return to gas absorption
System carries out gas absorption；Or the residual air after being absorbed through gas introduces residual air processing system, carries out 2~4 sodium hydroxides
Alkali liquor absorption treatment, collects absorbing liquid and obtains sodium sulfite Na2SO3Solution；Residual exhaust after being processed through residual air processing system is arranged
Go out system.
The method for extracting rhenium of the present invention, further, the extension diameter section is highly 3~6m, and undergauge section height is 1
~1.5m.
The method for extracting rhenium of the present invention, further, the rhenium-containing ore deposit is rich rhenium molybdenum concntrate, rhenium-containing amount >=
100g/t, it is 560~600 DEG C to control hybrid reaction area sintering temperature；Or the rhenium-containing ore deposit is rich rhenium brightness lindgrenite, rhenium-containing amount
>=100g/t, it is 600~700 DEG C to control hybrid reaction area sintering temperature.Preferably, when the rhenium-containing ore deposit is rich rhenium molybdenum concntrate
When, its rhenium-containing amount is in 1300~1900g/t；When the rhenium-containing ore deposit is rich rhenium brightness lindgrenite, its rhenium-containing amount is in 500~600g/t.
The method for extracting rhenium of the present invention, further, the dust pelletizing system includes 1-2 grades of whirlwind being sequentially connected
Deduster and ceramic element dust-precipitator, baking flue gas first pass through cyclone dust collectors dedusting, then are received by ceramic element dust-precipitator
Dirt.
The method for extracting rhenium of the present invention, further, the gas absorption system is provided with 1~2 grade of spray-absorption
Device and 1~2 grade of packing material absorbing device.
The method for extracting rhenium of the present invention, further, the residual air processes regeneration step, first with high-molecular porous
Sulfur dioxide of the microballoon in 5~35 DEG C of absorption residual air, then the porous polymer bead of adsorption saturation is passed through 130~155 DEG C
Hot blast desorption, obtain regenerate sulfur dioxide；Or in the residual air process step, first with the ealkaline buffer of addition organic amine
The sulfur dioxide in residual air is absorbed, then adsorption liquid is heated to 90~120 DEG C, obtain regenerating sulfur dioxide.
The method for extracting rhenium of the present invention, further, the oxygen-containing air is pure industrial oxygen and purify air
Gaseous mixture, or be purify air through the central hole structure sorbent circulation oxygen-containing air stream that obtains of absorption.
The method for extracting rhenium of the present invention, further, the dust or return oxygen obtained after the high-temperature dust removal
Change calcination stepses, or carry out Soaking treatment, during water logging, added under 40~60 DEG C of stirring sodium hypochlorite NaClO or
Hydrogen peroxide H2O2, and pH9~10 are adjusted, bubble-free occurs into solution, and the infusion being filtrated to get is incorporated to step（3）Contain
In rhenium extract solution.
Using the method for the present invention, extraction rhenium obtains rhenium-containing extract solution from rhenium-containing ore deposit, at least has the advantages that：
1st, the oxidizing roasting efficiency and rhenium volatility of rhenium-containing ore deposit are improve, roasting Dust Capacity is reduced, production effect is improve
Rate
The present invention sets extension diameter section and undergauge section by boiling furnace body second reaction zone, improves rhenium in rhenium-containing ore deposit
Oxidizing roasting efficiency, specifically, because conventional boiling furnace body is an isometrical cylindrical refractory chamber, rhenium-containing mineral aggregate connects with oxygen source
After touching mixing, constantly flowed up when the oxidation reaction of sulphide ore is carried out, after mixed material flows through discharging opening still in tempo
Degree is flowed up, it is difficult to ensure the oxidization time of sulfuration rhenium, and uses the inventive method, the hybrid reaction area below discharging opening
In, the main oxidation sweetening reaction that sulphide ore in rhenium-containing ore deposit occurs, sulfuration rhenium is almost not involved in reaction, aoxidize the calcining of generation from
Discharging opening is discharged, and remaining a small amount of unreacted sulphide ore, sulfuration rhenium are upwardly into second reaction zone together with flue gas, expanding
Section, rises material and flows up speed reduction, extends and ensure that residence time of the sulfuration rhenium in fluidized bed furnace, improves rhenium
Oxidizing roasting efficiency, improves rhenium volatility；When the rhenium oxide for aoxidizing generation flows upward through undergauge section, due to undergauge section
Presence, rise material channel narrows, flowing velocity increases, and can accelerate rhenium oxide that extension diameter section generated to upstream
It is dynamic, shorten newly-generated rhenium oxide and dust and the time of contact of sulfur dioxide, therefore, the present invention is anti-by set second
Area is answered, by extension diameter section and the integrated structure of undergauge section, the oxidizing roasting time of rhenium can either be controlled, turn avoid the rhenium of generation
Oxide, relative to the fluidized bed furnace of conventional isometrical cylindrical furnace, substantially increases the volatility of rhenium by the inverse reduction of sulfur dioxide；
And, in conventional fluidized bed furnace, flue gas carries dust and is flowed up by certain flow rate, and the dust that flue gas is carried has little time
Sedimentation is discharged by exhanst gas outlet, causes Dust Capacity excessive, and the present invention is hybrid reaction by by fluidized bed furnace Proper Design
Area and the second reaction zone structure with extension diameter section section thereon, when flue gas carries dust into extension diameter section, expanding effect makes dust
Ascent rate reduction, moves downward landing and enters hybrid reaction area under gravity, from discharging opening discharge, reduces rising cigarette
The Dust Capacity that gas is carried, reduces the Dust Capacity that stove is returned in roasting, and specific productivity is relative to be improved, and reduces entreprise cost；
Additionally, the present invention is by adjusting the coefficient of excess air and hybrid reaction area oxygen of oxygen-containing air during oxidizing roasting
Partial pressure, with reference to the setting of second reaction zone, makes the sulphide ore in rhenium-containing ore deposit be aoxidized more fully in hybrid reaction area, in reduction calcining
Sulfur content, and can make that the rhenium in rhenium-containing ore deposit is fully oxidized to be volatized into gaseous smoke, further improve the volatility of rhenium.
2nd, dedusting method and gas absorption system are improved, rhenium-containing flue gas is reduced in dedusting and gas absorption process
Loss
Rhenium oxide Re2O7Boiling point is 361 DEG C, rhenium-containing flue gas during solid dust is removed in separation, volatilization state
Re2O7It is easy to be mixed into the dust being trapped because of cooling, is also easily entered by the sulphur dioxide reduction in flue gas because lowering the temperature
In dust, the recycled in its entirety rate of rhenium, the present invention is influenceed to use high-temperature dust removal system, compared with conventional low temperature bag-type dust, energy
Hot conditions of the flue gas in dust removal process are enough kept, so as to rhenium oxide remains at gas shape in ensure that dust removal process
State, is prevented effectively from the rhenium loss in dust removal process, improves the rate of recovery of rhenium；
The present invention, by the pH value for keeping absorbing liquid higher, improves the absorptivity of rhenium in gas absorption process, it is to avoid
Liquid acidity is absorbed when directly being absorbed with clear water in conventional absorption mode and constantly increases the drawbacks of causing rhenium absorptivity constantly to decline, carried
The absorptivity of rhenium high, reduces the rhenium loss in absorption process, so as to improve the rate of recovery of rhenium.
3rd, the recycled in its entirety rate that oxidizing roasting mode extracts rhenium is improve, the fast development that rhenium extracts industry is promoted
In the method that existing oxidizing roasting mode reclaims rhenium, rhenium is merely possible to byproduct and is recycled, will
Rhenium in rhenium-containing mineral extracts the Rhenium recovery rate entered in rhenium-containing extract solution always in 60-70% or so, most of rhenium element conduct
Waste material is abandoned, and has had a strong impact on the recycling of the rhenium element of dilute scattered distribution itself；
It is rhenium oxide by the sulfuration rhenium oxidizing roasting in rhenium-containing ore deposit, is that oxidizing roasting mode carries out the of Rhenium recovery flow
One step, the oxidizing roasting efficiency and the height of volatility of rhenium, the height to Rhenium recovery rate in whole extraction process is most important, oxygen
Change roasting is more complete, and the volatility of rhenium is higher, it is meant that the rhenium remained in dust and calcining is fewer, enters into gas and finally
The rhenium for entering rhenium-containing extract solution is more, and rhenium extracts more complete, and the present invention is by improving fluidized bed furnace furnace binding and fluosolids roasting work
Skill parameter, makes the distillation volatility of rhenium bring up to almost 100%, and the rhenium oxide after volatilizing is by high-temperature dust removal mode and height
The gas absorption features of absorptivity, make the most rhenium elements in rhenium-containing ore deposit by after the absorption of oxidizing roasting, dedusting and gas
Into in rhenium-containing extract solution, the oxidizing roasting mode in industry that improves extracts the recycled in its entirety rate of rhenium, can aoxidize rhenium-containing ore deposit
The rate of recovery being calcined into rhenium-containing extract solution reaches more than 97%, promotes rhenium extraction and the fast development of rhenium application industry, realizes
Utilization of resources.
Brief description of the drawings
Fig. 1 is the process flow diagram of the embodiment of the present invention 1；
Fig. 2 is the process flow diagram of the embodiment of the present invention 2；
Fig. 3 is oxidizing roasting fluidized bed furnace concrete structure schematic diagram in embodiment 1 and embodiment 2.
In accompanying drawing：1st, body of heater；2nd, hybrid reaction area；3rd, discharging opening；4th, extension diameter section；5th, undergauge section；6th, exhanst gas outlet；7th, wind
Room；8th, air inlet pipe；9th, gas distribution separator；10th, charging aperture；α, base angle；β, drift angle.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment the present invention is further elaborated, but protection scope of the present invention include but do not limit
In this.
Embodiment 1：
The method for extracting rhenium of the invention, technological process is as shown in figure 1, comprise the technical steps that：
（1）Rhenium-containing ore deposit oxidizing roasting
Rhenium-containing ore deposit is sent into fluidized bed furnace, is contacted with oxygen-containing air and is calcined；Fluidized bed furnace concrete structure is as shown in figure 3, boiling
Rise stove bottom and be provided with gas distribution separator 9 i.e. furnace bottom with holes, be to be provided with the air compartment 7 of air inlet pipe 8 below furnace bottom, air inlet pipe 8 with
Air feed system is connected, and body of heater 1 at the upward 1.0~1.5m height of furnace bottom along being respectively equipped with charging aperture 10 and discharging opening 3, charging aperture
10 are slightly above discharging opening 3, and boiling furnace body 1 is provided with hybrid reaction area 2 and second reaction zone, and second reaction zone is higher than discharging opening 3
And extension diameter section 4 and undergauge section 5 are sequentially provided with upwards along body of heater 1, extension diameter section 4 is with the diameter of hybrid reaction area 2 than 1.1~1.8：1, expand
Footpath section 4 is truncated cone-shaped with the binding site of hybrid reaction area 2, and its vertical section is isosceles trapezoid, and the base angle of round platform is 15~30o, contracting
Footpath section 5 is with the diameter of hybrid reaction area 2 than 0.3~0.5：1, undergauge section 5 is truncated cone-shaped, its vertical section with the binding site of extension diameter section 4
It is isosceles trapezoid, the apex angle ss of round platform is 110~145o, and the outlet of undergauge section 5 is connected with the exhanst gas outlet 6 on body of heater 1；
In the specific implementation, rhenium-containing ore deposit can preferentially from rich rhenium molybdenum concntrate（That is molybdenite concentrate）, also can select richness rhenium brightness molybdenum
Copper mine（It is associated with the copper sulfide concentrate of molybdenum）, its rhenium-containing amount is held in more than 100g/t, i.e., per ton to feed rhenium element in ore deposit
Content is more than 100 grams；In the present invention, the rich rhenium ore deposit is the ore deposit of rhenium-containing amount >=100g/t；Conventional molybdenum concntrate rhenium-containing amount is 30
~40g/t, in 30~50g/t, the content of rhenium is low, and value is limited for conventional brightness lindgrenite rhenium-containing amount, and rhenium-containing amount >=100g/
The rich rhenium ore deposit of more than t, its rhenium enrichment degree is high, possesses more preferable actual recovered value；During specific implementation, preferential selection contains
Rhenium amount 1300~1900g/t rich rhenium molybdenum concntrate or rhenium-containing amount 500~600g/t rich rhenium brightness lindgrenite；The present embodiment
In, using rich rhenium molybdenum concntrate, its rhenium-containing amount is 1480 g/t to rhenium-containing ore deposit raw material；
During concrete operations, rhenium-containing ore deposit can first be crushed to the miberal powder of 200 mesh or so before fluidized bed furnace is sent into, also can be by powder
It is granulation into pelletizing shape to feed again, fluidization operation is carried out in fluidized bed furnace beneficial to mineral aggregate；During charging, rhenium-containing ore deposit can be carried using being provided with
The automatic feed system charging of the machine of liter, feed system is connected with charging aperture 10, can convey mineral aggregate by set amount uniformly continuous
Enter in fluidized bed furnace；
During oxidizing roasting, holdup time to mineral aggregate in stove of the structure of main reaction region fluidized bed furnace, rhenium enter flue gas
Volatility have extreme influence, different from the isometrical cylindrical refractory chamber of conventional boiling furnace body, the present invention is in second reaction zone
The extension diameter section 4 of setting, can extend rhenium oxidizing roasting reaction in the residence time of second reaction zone, so as to improve oxidizing roasting effect
Rate and rhenium volatility, extension diameter section 4 is with the diameter of hybrid reaction area 2 than 1.1~1.8：1st, base angle is in 15~30o scopes, Neng Goubao
Rational rhenium oxidizing roasting time is demonstrate,proved, when α is more than 30o, excessive 1.8 times more than the diameter of hybrid reaction area 2 of the diameter of extension diameter section 4
When, the extension of rhenium oxidizing roasting duration is excessive, not only can reduction production capacity, and generation rhenium oxide and dust time of contact
It is long, rhenium volatility is reduced on the contrary；The undergauge section 5 set on extension diameter section 4, can make the rhenium oxide for having volatilized as early as possible
Discharge boiling furnace body 1, shortens the time of contact of rhenium oxide and dust and sulfur dioxide, practice have shown that, when undergauge section 5 with it is mixed
The diameter of reaction zone 2 is closed than 0.3~0.5：1st, when apex angle ss is the scope of 110~145o, the rhenium oxide for having volatilized can be arranged quickly
Go out body of heater 1, also do not interfere with the fully oxidized roasting of rhenium in extension diameter section 4；In practice, preferably the height of extension diameter section 4 is in 3~6m, contracting
Footpath section 5 height in 1~1.5m, to obtain preferably oxidizing roasting effect；In the present embodiment, extension diameter section 4 is straight with hybrid reaction area 2
Compare 1.4 in footpath：1, base angle is 22o, and the height 4.5m of extension diameter section 4, undergauge section 5 compares 0.3 with the diameter of hybrid reaction area 2：1, apex angle ss is
130o, 5 height 1.1m of undergauge section；
During oxidizing roasting, the oxygen-containing air that being calcined needs can be using the mixing of pure industrial oxygen and purify air
Gas, it would however also be possible to employ purify air is through central hole structure adsorbent（If aperture is in the mesopore activated carbon or molecular sieve of 50~300Ao）
The oxygen-containing air stream that circulation absorption is obtained, the present embodiment carries out the oxidizing roasting of rhenium-containing ore deposit using the first oxygen-containing air；This hair
In bright, in roasting process, the coefficient of excess air of oxygen-containing air is controlled（That is amount of actual air for combustion and theoretical demand air capacity volume
The ratio between）It is 1.2~2.5%, 560~700 DEG C of hybrid reaction area sintering temperature, 23~180KPa of partial pressure of oxygen is aoxidized in rhenium-containing ore deposit and roasted
During burning, oxygen supply situation directly affects mineral oxide roasting efficiency and rhenium volatility in stove, and oxygen-containing air amount crosses conference reduction
Rhenium oxide concentration in flue gas, reduces flue-gas temperature, increases recovery difficult, reduces sulfur dioxide content in flue gas, increases
Purging sulfur dioxide intractability, oxygen-containing air amount is too small, then be difficult to ensure that roasting quality, causes flue-gas temperature too high, and rhenium is returned
Yield reduction, practice have shown that, control oxygen-containing air coefficient of excess air be 1.2~2.5% under the conditions of, rhenium-containing ore deposit can be realized
Oxygen-enriched air roasting, beneficial to improving conversion ratio of the sulfuration rhenium to rhenium oxide, during rhenium can obtain fully oxidized entrance flue gas in mineral；This
Outward, when partial pressure of oxygen is less than 23 KPa in hybrid reaction area, sulfur content is drastically raised in calcining, and the oxidizing roasting of rhenium can be influenceed to imitate
Rate, more than after 180KPa, the voloxidation efficiency influence on rhenium is not notable, can also cause oxygen source to waste for partial pressure of oxygen；In roasting
During rich rhenium molybdenite, under the conditions of hybrid reaction area sintering temperature is less than 560 DEG C, roasting is slow, manufacturing schedule is influenceed, higher than 600 DEG C
The molybdenum trioxide in molybdenum calcining can distil and be mixed into flue gas afterwards, increase the molybdenum content in the follow-up rhenium-containing extract solution for obtaining, and increase
Rhenium purifies pressure, therefore, during roasting, priority acccess control hybrid reaction area's sintering temperature is at 560~600 DEG C；The present embodiment control contains
The coefficient of excess air of oxygen air is 1.8%, 565 DEG C of hybrid reaction area sintering temperature, partial pressure of oxygen 130KPa；It is calcined the cigarette of generation
Gas carries dust and is discharged by exhanst gas outlet 6 through undergauge section 5, and calcining is discharged from discharging opening 3 and collected；
（2）Baking flue gas high-temperature dust removal
Baking flue gas are introduced into dust pelletizing system, in dust removal process, it is 405~450 to keep flue gas temperature in dust pelletizing system
DEG C, obtained after dedusting except dust and gas and dust；
The rhenium oxide and sulfur dioxide generated in oxidizing roasting step enter in flue gas together, while flue gas is carried again
The dust of inlet amount about 20%, when dust pelletizing system temperature is less than rhenium compound boiling point, the rhenium oxide of state of volatilizing not only can be because of cooling
It is mixed into dust, and the rate of recovery of rhenium by the sulphur dioxide reduction in flue gas into rhenium disulfide and rhenium salt, can be influenceed, puts into practice table
It is bright, keep flue gas when temperature in dust pelletizing system is more than 405 DEG C, rhenium oxide is positively retained at gaseous state, due to roasting cigarette
With the heat load problem of gas absorption system after heat loss, and consideration dedusting during gas introducing dust pelletizing system, keep
In dust pelletizing system temperature below 450 DEG C than convenient and economy；
During specific implementation, dust pelletizing system may include 1~2 grade of cyclone dust collectors being sequentially connected and ceramic element dust-precipitator,
Baking flue gas first pass through cyclone dust collectors dedusting, then are gathered dust by ceramic element dust-precipitator；Ceramic element dust-precipitator generally sets
There are housing, ceramic filter filter core, pulse cleaning system and soot cleaning system, during gathering dust, the fine grained in high-temperature roasting flue gas
Dust is gradually deposited in filter core outer surface and forms ash cake, and increasing pressure drop with ash cake thickness increases, and blowback system is in time to filter core
Blowback cleaning is carried out, is effectively removed and by dust collection in dust-precipitator bottom, realization is gathered dust online；In the present embodiment, dedusting system
System is provided with 1 grade of cyclone dust removal and ceramic element gathers dust, and ceramic element dust-precipitator housing is provided with heat-insulation layer, more preferably to ensure dedusting
The hot conditions of system；So, through above-mentioned steps（1）Oxidizing roasting generation rhenium oxide as flue gas a part, with row
The dust for going out fluidized bed furnace enters cyclone dust collectors, and after removing most of dust, rhenium-containing flue gas then carries fine dusts by ceramics
Filter core dust-precipitator, dust is retained down, and rhenium-containing gas is then turned into except dust and gas by filter core；
The dust obtained after high-temperature dust removal, still containing a small amount of unoxidized rhenium, it is necessary to further recycle, specifically
During operation, dust can be returned to oxidizing roasting step, rhenium therein is extracted in roasting again, it is also possible to dust is carried out at water logging
Reason, during water logging, adds NaClO or H under 40~60 DEG C of stirring2O2, and pH9~10 are adjusted, bubble-free goes out into solution
It is existing, there is at most muddiness, the rhenium-containing infusion that will be filtrated to get is incorporated to following step（3）Rhenium-containing extract solution in；The present embodiment
It is middle using by the dust after dedusting return stove baking modes reclaim dust in remaining rhenium；
（3）Rhenium oxide gas absorbs
Gas absorption system will be introduced except dust and gas, keep gas absorption system absorption liquid pH >=4, absorbed except the rhenium in dust and gas
Oxide and sulfur dioxide, obtain rhenium-containing extract solution and residual air；In gas absorption process, rhenium oxide and sulfur dioxide are inhaled
Take in extract solution, with the carrying out for absorbing, extracting liquid acidity increases, and pH declines, unfavorable to absorbing, practice have shown that, only adopt
The absorptivity for being difficult to maintain high is absorbed with clear water, when absorption liquid pH >=4 are kept, beneficial to being normally carried out that gas absorbs, is put into practice
On can to use the water of addition ealkaline buffer be absorbing liquid, such as to add the water of organic amine as absorbing liquid, raising absorptivity,
So as to except the rhenium oxide in dust and gas obtains fully absorbing into rhenium-containing extract solution, be convenient for the rhenium enriching and purifying of next step
Operation；During specific implementation, gas absorption system can be set 1~2 grade of spray-absorption device and 1~2 grade of packing material absorbing device, dedusting
After gas first absorbs through leacheate cooling, then it is enriched with by packing material absorbing device, collection obtains rhenium-containing extract solution；The present embodiment
Absorb and remove dust and gas using 1 grade of spray absorber and 1 grade of packed absorber series connection, and collect rhenium-containing extract solution；
During specific implementation, the rhenium-containing extract solution for obtaining, next step directly can prepare ammonium perrhenate or rhenium high by condensing crystallizing
Sour potassium, or first pass through the separation and concentration means such as organic solvent extraction, ion exchange, charcoal absorption and be further purified enrichment,
Perrhenic acid or potassium perrhenate product are prepared by condensing crystallizing again, also rhenium metal can further be produced by perrhenate；
（4）Residual air treatment
Residual air after being absorbed through gas, mainly contains unabsorbed sulfur dioxide, it is impossible to be directly discharged into air, otherwise
Environmental security can be influenceed, it is necessary to carry out residual air treatment, discharged again after meet the requirement of environmental protection；
The inventive method, the residual air after being absorbed through gas introduces residual air processing system, carries out residual air treatment regeneration or remaining
Gas disposal is removed；
Residual air processes regenerative process, and sulfur dioxide in residual air actually is carried out into separation and concentration recycling, specifically, can
Carried out with using absorption-desorption mode, during operation, the dioxy in first can adsorbing residual air at 5~35 DEG C with porous polymer bead
Change sulphur, then the porous polymer bead of adsorption saturation be passed through 130~155 DEG C of hot blast desorption, obtain regenerating sulfur dioxide,
The sulfur dioxide in residual air can be first absorbed with the ealkaline buffer of addition organic amine, then adsorption liquid is heated to 90~120 DEG C,
The regeneration sulfur dioxide of concentration raising is obtained, sulfur dioxide or return oxidizing roasting step after regeneration are mixed with oxygen-containing air
It is used for the oxidizing roasting of rhenium-containing ore deposit after conjunction, or return gas absorption system carries out gas absorption, forms the recovery of sulfur dioxide
Using circulation；So, the residual exhaust after being processed through regeneration can reach emission request；
And residual air treatment removal process, it is to absorb sulfur dioxide suitable sorbent in residual air, during operation, 2 can be carried out
The treatment of~4 sodium hydroxide alkali liquor absorptions, collects absorbing liquid and obtains sodium sulfite Na2SO3Solution, through the residual exhaust after absorption
Emission request can be reached；
The present embodiment is low at 20 DEG C using the polystyrene type porous polymer bead of particle diameter 1.0mm spherical particles
Sulfur dioxide is desorbed under the lower absorption of temperature, 135 DEG C of high temperature, and the sulfur dioxide that will be regenerated returns to calcination stepses, for rhenium-containing ore deposit
Oxidizing roasting, reaches the residual exhaust of emission request then safe discharge system.
From in terms of result of implementation, the oxidizing roasting richness rhenium molybdenum concntrate under above-mentioned implementation condition, rhenium is extracted back in oxidizing roasting step
Up to more than 99%, dust returns furnace volume less than 10% to yield, and the rhenium after being absorbed through two grades of rhenium oxides of high-temperature dust removal and spraying filler is returned
, up to 97.8%, the tail gas sulphur dioxide amount after treatment is in 50mg/m for yield3Hereinafter, extracted with existing rhenium and enter rhenium-containing extract solution
In Rhenium recovery rate 60~70% compare, substantially increase production efficiency, significantly improve oxidizing roasting mode and extract rhenium to rhenium-containing
The recycled in its entirety rate of extract solution.
Embodiment 2：
With rich rhenium brightness lindgrenite as raw material, the rhenium in mineral is extracted using oxidizing roasting mode, raw material rhenium-containing amount is 530g/
T, its technological process is as shown in Fig. 2 comprise the technical steps that：
（1）Rhenium-containing ore deposit oxidizing roasting
Rhenium-containing ore deposit raw material is sent into fluidized bed furnace, is contacted with oxygen-containing air and is calcined；Fluidized bed furnace concrete structure such as Fig. 3 institutes
Show, boiling furnace body 1 is provided with hybrid reaction area 2 and second reaction zone, second reaction zone is higher than discharging opening 3 and upward along body of heater 1
Extension diameter section 4 and undergauge section 5 are sequentially provided with, extension diameter section 4 compares 1.4 with the diameter of hybrid reaction area 2：1, extension diameter section 4 and hybrid reaction area 2
Binding site is truncated cone-shaped, and its vertical section is isosceles trapezoid, and the base angle of round platform is 22o, the height 4.5m of extension diameter section 4, undergauge section 5
Compare 0.3 with the diameter of hybrid reaction area 2：1, undergauge section 5 is truncated cone-shaped with the binding site of extension diameter section 4, and its vertical section is isosceles trapezoid,
The apex angle ss of round platform is 130o, and undergauge 5 height 1.1m of section, the outlet of undergauge section 5 is connected with the exhanst gas outlet 6 on body of heater 1；
During oxidizing roasting, the oxygen-containing air that being calcined needs uses purify air via hole diameter in 50~300Ao
The oxygen-containing air stream that porous molecular sieve circulation absorption is obtained, it is 2.0%, partial pressure of oxygen to control the coefficient of excess air of oxygen-containing air
100KPa, during specific implementation, to rich rhenium brightness lindgrenite, 600~700 DEG C of control hybrid reaction area sintering temperature neither influences oxygen
Change baked for producing progress, also do not result in follow-up rhenium extraction purification pressure, the present embodiment controls the hybrid reaction area sintering temperature to be
660℃；The flue gas carrying dust for being calcined generation is discharged through undergauge section 5 by exhanst gas outlet 6；Calcining discharges collection by discharging opening 3；
（2）Baking flue gas high-temperature dust removal
Baking flue gas are introduced into dust pelletizing system, dust pelletizing system is provided with 1 grade of cyclone dust removal and ceramic element gathers dust, dust removal process
In, it is 420 DEG C to keep flue gas temperature in dust pelletizing system, is obtained after dedusting except dust and gas and dust；
The dust that will be obtained after high-temperature dust removal, carries out Soaking treatment, during water logging, is added under 60 DEG C of stirring
H2O2, and pH9~10 are adjusted, bubble-free occurs into solution, at most muddiness occurs, and the rhenium-containing infusion that will be filtrated to get is incorporated to
Following step（3）Rhenium-containing extract solution in；
（3）Rhenium oxide gas absorbs
Gas absorption system will be introduced except dust and gas, gas absorption system is provided with 1 grade of spray-absorption device and connection thereafter
1 grade of packing material absorbing device, to organic amine is added in absorbing liquid, keep gas absorption system absorption liquid pH=4, absorb and remove dust and gas
In rhenium oxide and sulfur dioxide, obtain rhenium-containing extract solution and residual air；The rhenium-containing extract solution of collection can be extracted by organic solvent
After taking enrichment, condensing crystallizing prepares ammonium perrhenate；
（4）Residual air treatment
Residual air after being absorbed through gas, the treatment of 3 sodium hydroxide alkali liquor absorptions is carried out at 0~10 DEG C, is collected absorbing liquid and is obtained
Na2SO3Solution, the Na that absorption is obtained2SO3Low temperature crystallization generation Na is carried out at 5 DEG C of solution2SO3Crystal, divides in centrifugal device
From drying is gone moisture removal to reclaim and obtains Na2SO3Solid；Residual exhaust then discharge system.
From in terms of result of implementation, the oxidizing roasting richness rhenium brightness lindgrenite under above-mentioned implementation condition, rhenium is extracted in oxidizing roasting step
Up to 99.2%, dust returns furnace volume in 8.9%, the Rhenium recovery after being absorbed through two grades of rhenium oxides of high-temperature dust removal and spraying filler to the rate of recovery
, up to 98.2%, the tail gas sulphur dioxide amount after three-level absorption treatment is in 60mg/m for rate3Hereinafter, the high efficiency extraction of rhenium is realized.
Claims (9)
1. it is a kind of extract rhenium method, it is characterised in that：Methods described is comprised the technical steps that：
（1）Rhenium-containing ore deposit oxidizing roasting
Rhenium-containing ore deposit is sent into fluidized bed furnace, is contacted with oxygen-containing air and is calcined；The boiling furnace body（1）It is provided with hybrid reaction area
（2）And second reaction zone, the second reaction zone is higher than discharging opening（3）And along body of heater（1）It is sequentially provided with extension diameter section upwards（4）With
Undergauge section（5）, the extension diameter section（4）With hybrid reaction area（2）Diameter is than 1.1~1.8：1, extension diameter section（4）With hybrid reaction area
（2）Binding site is truncated cone-shaped, and its vertical section is isosceles trapezoid, and the base angle of round platform is 15~30o, the undergauge section（5）With it is mixed
Close reaction zone（2）Diameter is than 0.3~0.5：1, undergauge section（5）With extension diameter section（4）Binding site is truncated cone-shaped, and its vertical section is etc.
Waist is trapezoidal, and the apex angle ss of round platform is 110~145o, the undergauge section（5）Outlet and body of heater（1）On exhanst gas outlet（6）Connection；
During oxidizing roasting, it is 1.2~2.5% to control the coefficient of excess air of oxygen-containing air, hybrid reaction area sintering temperature 560~
700 DEG C, 23~180KPa of partial pressure of oxygen, the flue gas for being calcined generation carries dust through undergauge section（5）By exhanst gas outlet（6）Discharge；
（2）Baking flue gas high-temperature dust removal
Baking flue gas are introduced into dust pelletizing system, in dust removal process, it is 405~450 DEG C to keep flue gas temperature in dust pelletizing system, is removed
Obtained after dirt except dust and gas and dust；
（3）Rhenium oxide gas absorbs
Gas absorption system will be introduced except dust and gas, keep gas absorption system absorption liquid pH >=4, absorbed except the rhenium oxidation in dust and gas
Thing and sulfur dioxide, obtain rhenium-containing extract solution and residual air；
（4）Residual air treatment
Residual air after being absorbed through gas introduces residual air processing system, carries out residual air treatment regeneration, sulfur dioxide after regeneration or
Person returns to oxidizing roasting step, the oxidizing roasting of rhenium-containing ore deposit is used for after mixing with oxygen-containing air, or return to gas absorption system
Carry out gas absorption；Or the residual air after being absorbed through gas introduces residual air processing system, carries out 2~4 sodium hydroxide alkali lye
Absorption is processed, and is collected absorbing liquid and is obtained sodium sulfite solution；Residual exhaust discharge system after being processed through residual air processing system.
2. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The extension diameter section（4）Highly for 3~
6m, undergauge section（5）Highly it is 1~1.5m.
3. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The rhenium-containing ore deposit is rich rhenium molybdenum concntrate,
Rhenium-containing amount >=100g/t, it is 560~600 DEG C to control hybrid reaction area sintering temperature；Or the rhenium-containing ore deposit is rich rhenium brightness molybdenum copper
Ore deposit, rhenium-containing amount >=100g/t, it is 600~700 DEG C to control hybrid reaction area sintering temperature.
4. it is according to claim 3 it is a kind of extract rhenium method, it is characterised in that：The rhenium-containing ore deposit is rich rhenium molybdenum concntrate
When, its rhenium-containing amount is in 1300~1900g/t；When the rhenium-containing ore deposit is rich rhenium brightness lindgrenite, its rhenium-containing amount is in 500~600g/t.
5. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The dust pelletizing system includes being sequentially connected
1~2 grade of cyclone dust collectors and ceramic element dust-precipitator, baking flue gas first pass through cyclone dust collectors dedusting, then by ceramic element
Dust-precipitator is gathered dust.
6. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The gas absorption system is provided with 1~2
Level spray-absorption device and 1~2 grade of packing material absorbing device.
7. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The residual air processes regeneration step, first
Sulfur dioxide in adsorbing residual air at 5~35 DEG C with porous polymer bead, then the porous polymer bead of adsorption saturation is led to
Enter 130~155 DEG C of hot blast desorption, obtain regenerating sulfur dioxide；Or in the residual air process step, first with addition organic amine
Ealkaline buffer absorb sulfur dioxide in residual air, then adsorption liquid is heated to 90~120 DEG C, obtain regenerating sulfur dioxide.
8. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The oxygen-containing air is pure industrial oxygen
Or it is purify air through the central hole structure sorbent circulation oxygen-containing air stream that obtains of absorption with the gaseous mixture of purify air.
9. it is according to claim 1 it is a kind of extract rhenium method, it is characterised in that：The dust obtained after the high-temperature dust removal
Or oxidizing roasting step is returned, or Soaking treatment is carried out, during water logging, hypochlorous acid is added under 40~60 DEG C of stirring
Sodium or hydrogen peroxide, and pH9~10 are adjusted, bubble-free occurs into solution, and the infusion being filtrated to get is incorporated to step（3）Contain
In rhenium extract solution.
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| CN112522519B (en) * | 2020-12-04 | 2023-11-03 | 合肥工业大学 | Method for grading and recycling metal rhenium from tungsten-rhenium alloy scrap |
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