CN107541608A - A kind of melt carbothermy magnesium technique and refining magnesium system - Google Patents
A kind of melt carbothermy magnesium technique and refining magnesium system Download PDFInfo
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- CN107541608A CN107541608A CN201710508851.0A CN201710508851A CN107541608A CN 107541608 A CN107541608 A CN 107541608A CN 201710508851 A CN201710508851 A CN 201710508851A CN 107541608 A CN107541608 A CN 107541608A
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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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
- Y02P10/10—Reduction of greenhouse gas [GHG] emissions
- Y02P10/122—Reduction of greenhouse gas [GHG] emissions by capturing or storing CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to non-ferrous metallurgy technology field, and in particular to a kind of melt carbothermy magnesium technique and refining magnesium system.Melt carbothermy magnesium technique, including：Melting iron liquid processed, vacuumize, fill protective gas; by carbon dust, magnesia powder under the protection of appropriate argon gas; it is continuously introduced into the form of gas-solid mixture in vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and carbon monoxide；Cooling device is fed gas into, after cooling, obtains liquid magnesium；Remaining gas is separated, and protective gas recycles, and carbon monoxide enters gas collector, and incendivity is used to generate electricity.Melt carbothermy refines magnesium system, including：Vacuum reaction system, the condensation collection system being sequentially connected.The reduction reaction of technique carbon dust and magnesia powder of the present invention only needs 10s, the rate of recovery >=90% of magnesium, purity >=90% of magnesium, and iron liquid recycles, and realizes continuous production.
Description
Technical field
The invention belongs to non-ferrous metallurgy technology field, and in particular to a kind of melt carbothermy magnesium technique and refining magnesium system
System.
Background technology
Magnesium is the metallic element that reserves are extremely abundant in the earth, accounts for the 2.1%--2.7% of earth gross mass, China's storage
Amount is the maximum country of global magnesium resource reserves.At present, tens billion of tons have been verified.Magnesium and magnesium alloy have that proportion is small, and intensity is high,
Damping property is good, shock resistance, and machinability is good, and thermal conductivity is good, and recyclable recycling, environmental pollution is few, has excellent environment excellent
Gesture and performance advantage, it is applied widely, it is a kind of rare metal of reusable edible.Magnesium industry is greatly developed in China and complete
Ball has obvious resources advantage and the market advantage.
Magnesium refining method in the world mainly has electrolysis and the major class of thermal reduction two.Thermal reduction be using dolime as
Raw material, using Al, C or silicon as reducing agent, using iron as thermal conducting agent, magnesium metal is made in reduction-oxidation magnesium under elevated temperature in vacuo.From
So far, most magnesium worker processed is all around how to improve and improve reduction for Canadian skin river teaching inventive " Pidgeon process "
Phase, improve the technical problems such as magnesium rate and studied.CN104120282B Northeastern University Zhang Tingan et al. invented in 2014
A kind of " method of quick continuous refining magnesium ", the technical scheme of use is：Dispensing pelletizing, pelletizing calcining, by the high temperature ball after calcining
Group, it is continuously fed in closed high temperature reduction furnace without being cooled under argon gas protection, then enters in the argon gas atmosphere of flowing
Row high temperature reduction reacts, and reaction temperature is 1300-1600 DEG C, is continuously available high temperature magnesium vapor, and mixed with argon gas, shape
High temperature reduction furnace is continuously excluded into high-temperature gas mixture, while reducing slag, high temperature magnesium vapor is condensed to obtain magnesium metal.The method
Reaction speed is fast, and the recovery time, the rate of recovery of magnesium brought up to 88% in 90min.CN103882246B discloses a kind of vacuum
Magnesium smelting device and its method, are melted using by ferrosilicon, and method of magnesium oxide is blown into ferrosilicon liquation, reduce magnesium processed.Above-mentioned two
Kind method, has as a drawback that：(1) react after a period of time, it is necessary to by Si-Fe-SiO2Liquation, after long-time cools down, from
Taken out in reduction furnace, recharge raw material；(2) above two method makees reducing agent using silicon, and iron is thermal conducting agent, and silicon and iron exist
During reaction, silicon gradually be oxidized generation solid silica, silica melting point at 1650 DEG C or so, silica
Boiling point is at 2230 DEG C, and under the reaction conditions, silica mixes with iron, and with the continuous progress of reaction, silicon gradually decreases, and two
The output of silica is continuously increased, and iron liquid thermal conductivity gradually reduces, when parts by weight of the silicon in iron liquid are less than 30%, it is necessary to
Stop experiment, the iron liquid in reduction furnace and reducing slag are all removed, thereby result in the waste of thermal conducting agent iron, production cost is still
It is higher, and whole preparation process can only be referred to as " quick semicontinuous refining magnesium ".To sum up, silicon be reducing agent, iron be thermal conducting agent, reduction
Magnesia prepares magnesium metal, and because its reducing agent is solid, thermal conducting agent is liquid-solid phase, product is solid, thermal conducting agent is not joined in itself
With reaction, it can not but be separated with raw material and product, cause course of reaction to need continuously to supply thermal conducting agent, so, no matter
How the reaction carries out technological improvement, can not all realize that the continuous no consumption of thermal conducting agent uses, production cost is still higher, and is
Slag dumping can only realize semi-continuous production.
The reducing agent price of silicothermic process is higher, and thermal conducting agent can not reuse, and reduction with carbon obtains the side of magnesium metal
Method is paid attention to for people always.In the 1830's, the research on carbon thermal reduction magnesium is constantly being carried out always, but
Be be mostly with study the reaction mechanism of carbon thermal reduction magnesia magnesium progress research, and be essentially all laboratory carry out
, the not no relevant report on carbon thermal reduction magnesia magnesium industry so far.
The content of the invention
For shortcoming and defect existing for the production of existing magnesium-smelting silicothermic process and research institute, solve traditional silicon heat refining magnesium and deposited
Reduction cycle length, high energy consumption, the shortcomings of cost is high, the present invention provides that a kind of cost is low, energy consumption is low, production efficiency is high, energy
Enough continuous productions and green melt carbothermy magnesium technique and its refining magnesium system.
To realize above technical purpose, the technical scheme is that：
A kind of melt carbothermy magnesium technique, specific operating procedure are as follows：
Step (1)：In vacuum reaction stove, according to the capacity of vacuum reaction stove and the metered pig iron of ratio, make it molten
Change is in iron liquid, in 1200 DEG C of -1650 DEG C or so heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-10000Pa using vacuum extractor；
Step (3)：Argon gas is filled into vacuum reaction stove, while to vacuum reaction stove heat, protects iron liquid boiling, temperature
Hold at 1200-1650 DEG C, and argon gas is full of whole vacuum reaction stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate argon gas, it is continuously introduced into the form of gas-solid mixture
In vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and CO gas；
Step (5)：Magnesium vapor, CO gas and argon gas in step (4) are sent into cooling device, after cooling, obtained
Liquid magnesium；Contain argon gas, carbon monoxide and dust in remaining gas；
Step (6)：Argon gas, carbon monoxide and dust in step (5) are separated, argon gas recycles, carbon monoxide
Into gas collector, follow-up carbon monoxide is after burning, available for generating electricity.
Further, the vacuum reaction stove described in step (1)~(4) is vaccum sensitive stove or vacuum arc furnace ignition.
Further, in step (2), the absolute pressure in vacuum reaction stove maintains 40-100Pa, and reaction is more thorough.
Further, in step (3), described argon gas can also use nitrogen, helium, neon etc. to protect any one in gas
Replace.
Further, in step (4), described carbon dust is the pulvis that particle diameter is 0.05-0.3mm, phosphorus content 80%-
82%.
Further, in step (4), the fineness of described magnesia powder is 0.05-0.3mm, in described magnesia powder, is contained
Aoxidize magnesium amount >=90%.
Further, in step (4), described carbon dust and magnesia powder can be carried out in advance before vaccum sensitive stove is entered
Mix operation.
In melt carbothermy magnesium technique provided by the present invention, i.e., in step (4), iron liquid is that thermal conducting agent, carbon dust are also
Former agent, magnesium metal obtained by reduction-oxidation magnesium.Chemical reaction is：C(S)+MgO(S)=CO(g)+Mg(g), this endothermic heat of reaction, supercharging
Reaction, reduce reaction pressure and rise reaction temperature, reaction carry out to the right.In vacuum reaction stove, iron liquid is in liquid phase, carbon dust
It is solid phase with magnesia, reaction product is that carbon monoxide and magnesium vapor spontaneous can travel upward and out iron liquid, promotes reaction to the right
Carry out, reaction temperature of the invention is controlled at 1200 DEG C -1650 DEG C, and reaction is the endothermic reaction, is promoted reaction to carry out to the right, is promoted
Step (4) is thoroughly carried out to the right, and for whole reduction reaction time control in 10s, the rate of recovery of metal brings up to more than 90%.And
And in step (4), reaction raw materials are solid phase entirely, reaction product is gas phase entirely, does not have product residual in iron liquid, iron liquid is only
The spatially and thermally source of reaction is provided, iron liquid can be used continuously.In addition, heretofore described argon gas, there is following four effect：
(1) protection gas is served as, avoids product magnesium from being oxidized；(2) argon gas continuously enters iron liquid, by product magnesium vapor and an oxygen in flowing
Change carbon to carry away, substantially reduce the residence time of magnesium vapor and carbon monoxide in reaction interface, promote reaction to carry out to the right；
(3) a small amount of impurity is inevitably mixed with magnesium oxide powder, these a small amount of solid impurities, insoluble in iron liquid, in argon gas
Under motion, solid impurity is brought to iron liquid surface, solid impurity and gradually added up, overflowed automatically from slag-drip opening；(4) carbon thermal reduction oxygen
Change magnesium, reactant is all solid phase, how to improve solid carbon and the frequency of phase oxidative magnesium contact, is always to restrict solid phase reaction speed
The principal element of rate, the present invention in the presence of appropriate argon gas, are changed into vapor solid, solid when raw material enters vacuum reaction stove
Thus, the contact frequency of carbon and magnesia is substantially increased in the gas phase in motion state is scattered, greatly improve reaction speed
Rate.Therefore, melt carbothermy magnesium technique provided by the invention, reaction is thorough, and reaction rate is high, residual without product in iron liquid
Stay, do not pollute iron liquid, iron liquid can be used with serialization, entirely be reacted under equipment fault-free conditions, it is possible to achieve sustained continuous
Metaplasia is produced.
The invention also discloses a kind of melt carbothermy to refine magnesium system, and the system includes the vacuum reaction system being sequentially connected
System, condensation collection system；
Described vacuum reaction system includes vacuum reaction stove, including vacuum reaction stove top case and vacuum reaction furnace body with
And necessary vacuum extractor, charge door, detection mouth and magnesium vapor delivery pipe are provided with vacuum reaction stove top case, it is anti-in vacuum
Answer and the first excessive cinder notch is provided with furnace body；Described the first conveying pipeline and the second conveying pipeline is placed in vacuum reaction by charge door
In stove, and the mouth of pipe of the first conveying pipeline and the second conveying pipeline is placed in iron liquid, and first is connected with the first described conveying pipeline
Admission line, the second admission line is connected with the second described gas pipeline；
Described condensation collection system, including magnesium vapor delivery pipe, the one-level cooling device that is connected with magnesium vapor delivery pipe, with
The connected deduster of one-level cooling device, the magnesium vapor bogey being connected with one-level cooling device and magnesium vapor bogey
Connected magnesium vapor condensing trapping device, magnesium vapor condensing trapping device bottom discharge mouth are connected with magnesium metal liquid tank, and magnesium steams
Gas condensing trapping device upper part discharge port is connected with the second deduster, and gas separator, gas are provided with the top of the second deduster
The discharging opening of body separator is connected with air accumulator and carbon monoxide air accumulator respectively.
As an improvement, described vacuum reaction stove is vaccum sensitive stove or vacuum arc furnace ignition.
As an improvement, described vacuum reaction system, in addition to it is arranged on the lowering or hoisting gear of vacuum reaction stove top case.
As an improvement, the mouth of pipe of the first conveying pipeline of described vacuum reaction system is also associated with the first injection rifle, second
The mouth of pipe of conveying pipeline is also associated with the second injection rifle, and the first injection rifle and the second muzzle for being blown rifle are placed in iron liquid, described
First conveying pipeline is connected with carbon dust storage warehouse, and second conveying pipeline is connected with magnesia storage warehouse.
As an improvement, described vacuum reaction system also includes slag collection system, described slag collection system include receiving slag ladle and
With receiving the waste residue conveying device that is connected of slag ladle, vacuum reaction stove is connected by first cinder notch that overflows with receipts slag ladle, and receipts slag ladle passes through the
Two excessive cinder notch are connected with waste residue conveying device, and valve is provided with the first excessive cinder notch and the second excessive cinder notch.Described waste residue is defeated
The bottom of device is sent to be provided with mobile device.
As an improvement, the bottom of the second described deduster is provided with dust discharge valve and vavuum pump.
As an improvement, offer floss hole in described magnesium metal liquid tank.
Compared with prior art, a kind of melt carbothermy magnesium technique disclosed by the invention and refining magnesium system, have such as
Lower innovative point：(1) compared with traditional magnesium-smelting silicothermic process technology, the present invention is relative to the technological requirement of the vacuum of vacuum system
It is not harsh.The present invention control vacuum reaction stove in absolute pressure maintain 40-100Pa, be because：If in vacuum reaction stove
Gaseous pressure is higher, can cause to liquid phase partial pressure increases in iron liquid in vacuum reaction stove, and then increase and magnesium vapor and one are aoxidized
The resistance of carbon, in order to accelerate magnesium vapor and carbon monoxide from the spilling speed in iron liquid (or iron phase), reduce vacuum reaction stove
Interior gaseous pressure, reaction can be made more thorough, improve reaction rate.
(2) reaction raw materials of the invention are carbon dust and magnesia powder, theoretically, melt carbothermy provided by the invention
Magnesium technique processed and refining magnesium system, relatively low to the purity and fineness requirement of raw material, it is the powder that particle diameter is 0.05-0.3mm to control carbon dust
Agent, phosphorus content 80%-82%, the fineness for controlling magnesia powder are 0.05-0.3mm, and magnesium amount >=90% containing oxidation is to make
Conversion ratio >=90% and purity be >=90% magnesium, i.e. raw material magnesia powder is converted into conversion ratio >=90% of magnesium, product magnesium
Purity >=90%, sometimes the purity of product magnesium can reach 95%, even more high.
(3) method provided by the invention is because high temperature reduction process entered in the inertia of flowing other argon gas atmosphere environment
OK, the argon gas that the high temperature magnesium vapor of generation is flowed continuously is taken away, in actual production, the technique control to the vacuum of vacuum system
System is not relatively harsh.Most of all, the technical scheme disclosed in CN104120282B reduces using Si-Fe, this area
Technical staff known in, Si is converted into silica (SiO during reduction reaction2), the SiO in vacuum reaction stove2It is solid
Phase, it is trapped in as reaction product in iron liquid, causes SiO in iron liquid2Content constantly increase, as SiO in iron liquid2Content surpass
When 70%, the mobility of whole iron liquid becomes extremely slowly, not continuing to react, and can only shut down, by whole vacuum reaction stove
Interior iron liquid all renews, so CN104120282B can not fully achieve continuous production.Technical scheme disclosed in the present application is adopted
Reducing agent is made with C (Fe), at the operational, reaction product is gas entirely, does not have the delay of reaction product in iron liquid, can not
The reaction trace impurity waste residue avoided is floated in iron liquid, reaches the first excessive cinder notch, automatic to overflow, so, allow in experimental facilities
Under conditions of, whole iron liquid can really realize continuous production with indefinite use.Control reaction time of the present invention exists
Within 10s, often producing the cost of material of 1 ton of magnesium metal only includes the cost of material of magnesia powder and carbon dust, and the cost of iron liquid can
To ignore, environmental protection, the novel environment-friendly process of energy-conservation are really realized.
(4) method provided by the invention, argon gas can recycle as protective gas after separation, vacuum reaction stove
Volume size can be with reasonable selection according to yield.
Brief description of the drawings
Fig. 1 is the structural representation of melt carbothermy refining magnesium system of the present invention.
Reference：1. the first conveying pipeline, 2. second conveying pipelines, 3. vacuum reaction stoves, 4. receipts slag ladles, 5. dedusters, 6.
One-level cooling device, 7. magnesium vapor bogeys, 8. magnesium vapor condensing trapping devices, 9. second dedusters, 10. second air inlet pipe
Road, 11. first admission lines, 12. magnesium metal liquid tanks, 13. air accumulators, 14. carbon monoxide air accumulators, 15. carbon dust storage warehouses,
16. magnesia storage warehouse, 17. waste residue conveying devices, 18. gas separators, 121. floss holes, 171. mobile devices, 301. is true
Sky reaction stove top case, 302. vacuum reaction furnace bodies, 303. charge doors, 304. detection mouths, 305. magnesium vapor delivery pipes, 3061.
First excessive cinder notch, 3062.Second excessive cinder notch, 307. iron liquids, 308 first injection rifles, 309 second injection rifles, 310. lowering or hoisting gears,
901. dust discharge valves, 902. vavuum pumps.
Embodiment
In following examples：
The fineness of used magnesia powder is 0.05-0.3mm, in described magnesia powder, magnesium amount >=90% containing oxidation.
Described carbon dust is the pulvis that particle diameter is 0.05-0.3mm, phosphorus content 80%-82%.
Used protection gas is the high-purity gas of purity >=99.9%.
To produce 50000 tons of magnesium per year to count, the volume of vacuum reaction stove (vaccum sensitive stove or vacuum arc furnace ignition) is 7-8 cubes
Rice, the weight of the iron of heating is 40 tons or so, and the dosage of required magnesia powder is about 90,000 tons, and carbon dust dosage is about 1.6 ten thousand
Ton.Used protection gas, by taking argon gas as an example, one ton of magnesium of production is, it is necessary to 100m3, pressure be 8-10kg/L argon gas, according to it
His protection gas, dosage are identical with argon gas dosage.
Described carbon dust and the temperature of magnesia powder can be normal temperature, can also pass through and be heated to be a little higher than room temperature in advance
Temperature.
Reaction described here cycle, also referred to as recovery time, refer to carbon dust and magnesia powder in vacuum reaction stove
Residence time.
Embodiment 1
A kind of melt carbothermy magnesium technique, specific operating procedure are as follows：
Step (1)：In vacuum reaction stove, according to the capacity of vacuum reaction stove and the metered pig iron of ratio, make it molten
Change is in iron liquid, in 1200 DEG C of -1650 DEG C or so heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-10000Pa using vacuum extractor；
Step (3)：Argon gas is filled into vacuum reaction stove, while to vacuum reaction stove heat, protects iron liquid boiling, temperature
Hold at 1200-1650 DEG C, and argon gas is full of whole vacuum reaction stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate argon gas, it is continuously introduced into the form of gas-solid mixture
In vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and carbon monoxide；
Step (5)：Gas in step (4) is sent into cooling device, after cooling, obtains liquid magnesium；Contain in remaining gas
There are argon gas, carbon monoxide and impurity (mainly dust)；
Step (6)：By the residual gas in step (5)：Argon gas, carbon monoxide and dust are separated, argon gas recovery profit
With carbon monoxide enters gas collector.(CO gas after burning, available for generate electricity)
Further, the vacuum reaction stove described in step (1)~(4) is vaccum sensitive stove, and the induction furnace is Medium frequency induction
Stove.
Embodiment 2
A kind of melt carbothermy magnesium technique, specific operating procedure are as follows：
Step (1)：In vacuum reaction stove, according to the capacity of vacuum reaction stove and the metered pig iron of ratio, make it molten
Change is in iron liquid, in 1200 DEG C of -1650 DEG C or so heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-100Pa using vacuum extractor；
Step (3)：Nitrogen is filled into vacuum reaction stove, while to vacuum reaction stove heat, protects iron liquid boiling, temperature
Hold at 1200-1650 DEG C, and nitrogen is full of whole vacuum reaction stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate nitrogen, it is continuously introduced into the form of gas-solid mixture
In vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and carbon monoxide；
Step (5)：Gas in step (4) is sent into cooling device, after cooling, obtains liquid magnesium；Contain in remaining gas
There are nitrogen, carbon monoxide and dust；
Step (6)：By the residual gas in step (5)：Nitrogen, carbon monoxide and dust are separated, nitrogen recycling profit
With carbon monoxide enters gas collector.(CO gas after burning, available for generate electricity)
Further, the vacuum reaction stove described in step (1)~(4) is vacuum arc furnace ignition.
Embodiment 3
A kind of melt carbothermy magnesium technique, specific operating procedure are as follows：
Step (1)：In vacuum reaction stove, according to the capacity of vacuum reaction stove and the metered pig iron of ratio, make it molten
Change is in iron liquid, in 1200 DEG C of -1650 DEG C or so heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-100Pa using vacuum extractor；
Step (3)：Helium is filled into vacuum reaction stove, while to vacuum reaction stove heat, protects iron liquid boiling, temperature
Hold at 1200-1650 DEG C, and nitrogen is full of whole vaccum sensitive stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate helium, it is continuously introduced into the form of gas-solid mixture
In vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and carbon monoxide；
Step (5)：Gas in step (4) is sent into cooling device, after cooling, obtains liquid magnesium；Contain in remaining gas
There are helium, carbon monoxide and dust；
Step (6)：By the residual gas in step (5)：Helium, carbon monoxide and dust are separated, helium recovery profit
With carbon monoxide enters gas collector.(CO gas after burning, available for generate electricity)
Further, the vacuum reaction stove described in step (1)~(4) is vaccum sensitive stove.
Embodiment 4
A kind of melt carbothermy magnesium technique, specific operating procedure are as follows：
Step (1)：In vacuum reaction stove, according to the capacity of vacuum reaction stove and the metered pig iron of ratio, make it molten
Change is in iron liquid, in 1200 DEG C of -1650 DEG C or so heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-100Pa using vacuum extractor；
Step (3)：Neon is filled into vacuum reaction stove, while to vacuum reaction stove heat, protects iron liquid boiling, temperature
Hold at 1200-1650 DEG C, and neon is full of whole vaccum sensitive stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate neon, it is continuously introduced into the form of gas-solid mixture
In vacuum reaction stove under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, it is main to produce magnesium vapor and carbon monoxide；
Step (5)：Gas in step (4) is sent into cooling device, after cooling, obtains liquid magnesium；Contain in remaining gas
There are neon, carbon monoxide and dust；
Step (6)：By the residual gas in step (5)：Neon, carbon monoxide are separated, and neon recycles, an oxygen
Change carbon and enter gas collector.(CO gas after burning, available for generate electricity)
Further, the vacuum reaction stove described in step (1)~(4) is vaccum sensitive stove.
Embodiment 5
A kind of melt carbothermy refines magnesium system, and the system includes vacuum reaction system, the condensation collection system being sequentially connected；
Described vacuum reaction system includes vacuum reaction stove 3, including vacuum reaction stove top case 301 and vacuum reaction stove stove
Body 302 and necessary vacuum extractor, (set on vacuum reaction stove top case 301 provided with charge door 303 on vacuum reaction stove 3
Multiple charge doors are equipped with, such as enter the charge door of iron liquid, enters the charge door of carbon dust, enter the charge door of magnesia powder, be referred to as feeding
Mouthfuls 303, do not list one by one herein), detection mouth 304 and magnesium vapor delivery pipe 305, be provided with first on vacuum reaction furnace body
Overflow cinder notch 3061；Described the first conveying pipeline 1 and the second conveying pipeline 2 is placed in vacuum reaction stove 3 by charge door 303, and the
The mouth of pipe of one conveying pipeline 1 and the second conveying pipeline 2 is placed in iron liquid 307, and the first air inlet is connected with the first described conveying pipeline 1
Pipeline 11, the second admission line 10 is connected with the second described gas pipeline 2；
Described condensation collection system, including magnesium vapor delivery pipe 305, the one-level that is connected with magnesium vapor delivery pipe 305 cooling
Device 6, the deduster 5 being connected with one-level cooling device 6, the magnesium vapor bogey 7 and magnesium being connected with one-level cooling device 6
The connected magnesium vapor condensing trapping device 8 of steam bogey 7, the bottom discharge mouth of magnesium vapor condensing trapping device 8 and magnesium metal
Liquid tank 12 is connected, and the upper part discharge port of magnesium vapor condensing trapping device 8 is connected with the second deduster 9, the top of the second deduster 9
Gas separator 18 is provided with, the discharging opening of gas separator 18 is connected with air accumulator 13 and carbon monoxide air accumulator 14 respectively.
As an improvement, described vacuum reaction stove uses vaccum sensitive stove or vacuum arc furnace ignition.
The operation principle of above-mentioned melt carbothermy refining magnesium system is：Iron is added into vacuum reaction stove 3 by charge door 303
Powder, gradually heating heating, 1200 DEG C -1650 DEG C are warming up to by temperature, iron powder is all melted, and insulation is standby, using vacuumizing
The absolute pressure value of vacuum reaction stove is maintained 40-100Pa by device；Then the filling protection gas into vacuum reaction stove, simultaneously
Persistently to vacuum reaction stove heat, iron liquid boiling, temperature is set to be maintained at 1200-1650 DEG C, and protect gas to be full of whole vacuum sense
Answer stove；Open the valve on the first admission line 11 and the second admission line 10, open the first conveying pipeline 1 of conveying carbon dust and defeated
The valve on the second conveying pipeline 2 of magnesia powder is sent, so, the gas-solid mixing of carbon dust-protection gas is formed in the first conveying pipeline 1
Thing, the gas-solid mixture of magnesia powder-protection gas, the gas-solid mixture and oxygen of carbon dust-protection gas are formed in the second conveying pipeline 2
The gas-solid mixture for changing magnesium powder-protection gas enters the iron of vacuum reaction stove 3 respectively along the first conveying pipeline 1 and the second conveying pipeline 2
In liquid 307, reduction reaction is carried out in iron liquid 307, caused magnesium vapor and CO gas protect gas along magnesium with part
Vapor pipe 305 enters follow-up condensation collection system；In collection system is condensed, magnesium vapor, CO gas and portion
After code insurance protects gas along magnesium vapor delivery pipe 305 into the removing dust of deduster 305, into one-level cooling device 6, enter after cooling
After entering the further cooling of magnesium vapor bogey 7, into magnesium vapor condensing trapping device 8, in magnesium vapor condensing trapping device 8
Interior, magnesium vapor is condensed into magnesium liquid, realize, CO gas and part protection gas in magnesium vapor condensing trapping device 8 only
Cool down uncooled, so as to realize the separation of magnesium vapor and CO gas and part protection gas, magnesium liquid relies on Action of Gravity Field
The bottom of magnesium vapor condensing trapping device 8 is collected at, metal magnesium liquid is entered by the discharging opening of magnesium vapor condensing trapping device 8
Tank 12, carbon monoxide and part protection gas after cooling, into after the dedusting of the second deduster 9, into (the gas of gas separator 18
Separator 18 can be absorption-desorption separator, or condensation separator or other gas separators, herein to gas point
Species and model from device do not limit, as long as can realize CO gas and protect the separation of gas), through separation
Afterwards, CO gas enters carbon monoxide air accumulator 14, protection gas recycles into air accumulator 13.
As an improvement, described vacuum reaction system, in order to facilitate the maintenance of vacuum reaction stove 3, charging, in vacuum reaction
On stove 3 lowering or hoisting gear 310 is provided with lid.
As an improvement, vacuum reaction stove 3 is entered by the first conveying pipeline 1, the second conveying pipeline 2 in order to increase gas-solid mixture
When speed, the mouth of pipe of the first conveying pipeline 1 and the second conveying pipeline 2 not directly enters vacuum reaction stove 3, but in the first conveying pipeline
1 mouth of pipe is also associated with the first injection rifle 308, and the mouth of pipe of the second conveying pipeline 2 is also associated with the second injection rifle 309, the first injection
The muzzle that rifle 308 and second is blown rifle 309 is placed in iron liquid, and (gun body that the first injection rifle 308 and second is blown rifle 309 should
Long enough, entered by charge door in vacuum reaction stove 3, part gun body is placed in vacuum reaction stove 3, part gun body is exposed at very
Outside empty reacting furnace 3) first injection rifle 308 and second be blown rifle on be additionally provided with necessary control valve, these control valves set
In the gun body being exposed at outside vacuum reaction stove 3, convenient control；First conveying pipeline 1 is connected with carbon dust storage warehouse 15, described
Second conveying pipeline is connected with magnesia storage warehouse 16, and necessary valve is provided between the storage tank 1 of carbon dust storage warehouse 15 and first
Door and control instrument.
As an improvement, carbon dust and magnesia powder are realized and mixed, it is sent into very by charge door 303 by the first conveying pipeline 1
307 times progress reduction reactions of iron liquid of empty reacting furnace 3.
As an improvement, because raw material is carbon dust and magnesia powder, inevitably contain in carbon dust and magnesia powder
The solid impurity of reaction is not involved in, when carbon dust and magnesia powder after the reaction in vacuum reaction stove 3, remaining solid impurity particle
With ascending air (magnesium vapor, CO gas and protection gas move the air-flow of formation upwards) motion upwards, finally due to
Action of Gravity Field swims in the surface of iron liquid 307, and after prolonged accumulation, being formed on iron liquid surface has certain thickness solid
Impurity, the presence of these solid impurities, resistance can be produced to ascending air, so, described vacuum reaction system also includes receiving
Slag system, described slag collection system include the waste residue conveying device 17 received slag ladle 4 and be connected with receiving slag ladle 4, and vacuum reaction stove 3 is logical
Cross the first excessive cinder notch 3061 with receiving slag ladle 4 to be connected, receive slag ladle 4 and be connected by the second excessive cinder notch 3062 with waste residue conveying device 17,
Necessary valve is provided with the first excessive excessive cinder notch 3062 of cinder notch 3061 and second.The bottom of described waste residue conveying device 17
Mobile device is also provided with, facilitates the movement of waste residue conveying device.During slag dumping, close second and overflow cinder notch 3062, open the
One excessive cinder notch 3061, solid impurity particle, cinder notch 3061 is overflow into slag ladle 4 is received along first, slag dumping finishes, and closes the first excessive slag
Mouth 3061.
As an improvement, the bottom of the second described deduster 9 is provided with dust discharge valve 901 and vavuum pump 902.Dust discharge valve
901 effect is the dust in the second deduster 9 of convenient discharge, and the main function of vavuum pump 902 realizes the second deduster 9
Vacuumizing.
As an improvement, offer floss hole 121 in described magnesium metal liquid tank 12.Set floss hole 121 purpose be,
Facilitate the magnesium metal in magnesium metal liquid tank 12 to overflow, into follow-up further processing step, such as metallic magnesium refining or be made
Magnesium products.
As an improvement, necessary valve and instrument should be installed in melt carbothermy of the present invention refines magnesium system.
In addition, according to the common knowledge of this area, vacuum reaction stove 3 should be connected with necessary vacuum extractor,
In practical operation, the fineness and particle diameter of magnesia powder and carbon dust are not limited to above-mentioned fineness and particle diameter, phosphorus content and
The parameter of magnesium content can also carry out reasonable selection fineness, particle diameter and purity according to this area's cost price.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical scheme described by inventive embodiments.It will be understood by those within the art that still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect, as long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of melt carbothermy magnesium technique, it is characterised in that specific operating procedure is as follows：
Step (1)：In vacuum reaction stove, the pig iron is added, it is in iron liquid to make its fusing, in 1200 DEG C of -1650 DEG C of heat preservation for standby use；
Step (2)：The absolute pressure value of vacuum reaction stove is maintained by 40-10000Pa using vacuum extractor；
Step (3)：Argon gas is filled into vacuum reaction stove, while to vacuum reaction stove heat, is maintained at iron liquid boiling, temperature
1200-1650 DEG C, and argon gas is full of whole vacuum reaction stove；
Step (4)：By carbon dust, magnesia powder under the protection of appropriate argon gas, vacuum is continuously introduced into the form of gas-solid mixture
In reacting furnace under the liquid level of iron liquid, reduction reaction is carried out in iron liquid, produces magnesium vapor and CO gas；
Step (5)：Magnesium vapor, CO gas and argon gas in step (4) are sent into cooling device, after cooling, obtain liquid
Magnesium；Remaining gas is argon gas, carbon monoxide and dust；
Step (6)：Argon gas, carbon monoxide and dust in step (5) are separated, argon gas recycles, and carbon monoxide enters
Gas collector.
2. a kind of melt carbothermy magnesium technique according to claim 1, it is characterised in that described in step (1)~(4)
Vacuum reaction stove be vaccum sensitive stove or vacuum arc furnace ignition.
A kind of 3. melt carbothermy magnesium technique according to claim 1, it is characterised in that in step (2), vacuum reaction
Absolute pressure in stove maintains 40-100Pa.
A kind of 4. melt carbothermy magnesium technique according to claim 1, it is characterised in that in step (3), described argon
Any one in gas nitrogen, helium, neon is replaced.
A kind of 5. melt carbothermy magnesium technique according to claim 1, it is characterised in that in step (4), described carbon
Powder is the pulvis that particle diameter is 0.05-0.3mm, phosphorus content 80%-82%.
A kind of 6. melt carbothermy magnesium technique according to claim 1, it is characterised in that in step (4), described oxygen
The fineness for changing magnesium powder is 0.05-0.3mm；In described magnesia powder, magnesium amount >=90% containing oxidation.
7. a kind of melt carbothermy refines magnesium system, it is characterised in that the system includes the vacuum reaction system being sequentially connected and cold
Solidifying collection system, described vacuum reaction system also include slag collection system；
Described vacuum reaction system includes vacuum reaction stove (3), including vacuum reaction stove top case (301), vacuum reaction stove stove
Body (302) and vacuum extractor, charge door (303), detection mouth (304) and magnesium steaming are provided with vacuum reaction stove top case (301)
Letter shoot (305), the first excessive cinder notch (3061) is provided with vacuum reaction furnace body；Described the first conveying pipeline (1) and
Second conveying pipeline (2) is placed in vacuum reaction stove (3) by charge door (303), and the first conveying pipeline (1) and the second conveying pipeline
(2) the mouth of pipe is placed in iron liquid (307), the first admission line (11) is connected with described the first conveying pipeline (1), described
The second gas pipeline (2) on be connected with the second admission line (10)；
Described slag collection system includes the waste residue conveying device (17) received slag ladle (4) and be connected with receiving slag ladle (4), vacuum reaction stove
(3) it is connected by the first excessive cinder notch (3061) with receiving slag ladle (4), it is defeated by the second excessive cinder notch (3062) and waste residue receives slag ladle (4)
Send device (17) to be connected, valve is provided with the first excessive cinder notch (3061) and the second excessive cinder notch (3062)；
Described condensation collection system, including magnesium vapor delivery pipe (305), the one-level that is connected with magnesium vapor delivery pipe (305) cooling
Device (6), the deduster (5) being connected with one-level cooling device (6), the magnesium vapor carrying dress being connected with one-level cooling device (6)
Put (7), the magnesium vapor condensing trapping device (8) being connected with magnesium vapor bogey (7), magnesium vapor condensing trapping device (8) bottom
Portion's discharging opening is connected with magnesium metal liquid tank (12), magnesium vapor condensing trapping device (8) upper part discharge port and the second deduster (9)
Be connected, be provided with gas separator (18) at the top of the second deduster (9), the discharging opening of gas separator (18) respectively with gas storage
Tank (13) is connected with carbon monoxide air accumulator (14).
A kind of 8. melt carbothermy refining magnesium system according to claim 7, it is characterised in that described vacuum reaction stove
(301) it is vaccum sensitive stove or vacuum arc furnace ignition.
A kind of 9. melt carbothermy refining magnesium system according to claim 7, it is characterised in that described vacuum reaction system
The mouth of pipe of the first conveying pipeline (1) be also associated with the first injection rifle (308), the mouth of pipe of the second conveying pipeline (2) is also associated with second
Rifle (309) is blown, the first injection rifle (308) and the second muzzle for being blown rifle (309) are placed in iron liquid (307), and described first
Conveying pipeline (1) is connected with carbon dust storage warehouse (15), and second conveying pipeline (2) is connected with magnesia storage warehouse (16).
A kind of 10. melt carbothermy refining magnesium system according to claim 7, it is characterised in that first conveying pipeline (1)
It is same feed pipe with the second conveying pipeline (2), described same feed pipe is used for the mixture for conveying carbon dust and magnesia, in institute
On the same feed pipe stated, admission line is connected with.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610495930.8A CN106011500A (en) | 2016-06-29 | 2016-06-29 | Molten carbon heating type induction furnace based vacuum magnesium production system and magnesium production method thereof |
| CN2016104959308 | 2016-06-29 |
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| CN107541608A true CN107541608A (en) | 2018-01-05 |
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| CN201610495930.8A Pending CN106011500A (en) | 2016-06-29 | 2016-06-29 | Molten carbon heating type induction furnace based vacuum magnesium production system and magnesium production method thereof |
| CN201710508851.0A Pending CN107541608A (en) | 2016-06-29 | 2017-06-28 | A kind of melt carbothermy magnesium technique and refining magnesium system |
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| CN201610495930.8A Pending CN106011500A (en) | 2016-06-29 | 2016-06-29 | Molten carbon heating type induction furnace based vacuum magnesium production system and magnesium production method thereof |
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| WO (1) | WO2018001265A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111270088A (en) * | 2020-02-10 | 2020-06-12 | 中国恩菲工程技术有限公司 | System and method for continuously smelting magnesium by induction heating liquid stirring |
| CN112609091A (en) * | 2020-12-28 | 2021-04-06 | 金先奎 | Method for smelting magnesium metal by carbothermic reduction |
| WO2021121312A1 (en) * | 2019-12-17 | 2021-06-24 | 郑州大学 | Method for carbothermic smelting of magnesium and co-production of calcium carbide |
| CN114737057A (en) * | 2022-03-24 | 2022-07-12 | 东北大学 | Method for preparing high vapor pressure metal by carbothermic reduction |
| CN114870568A (en) * | 2022-03-24 | 2022-08-09 | 东北大学 | Device for smelting active high-vapor-pressure metal by carbon thermal reduction and using method thereof |
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| CN106011500A (en) * | 2016-06-29 | 2016-10-12 | 狄保法 | Molten carbon heating type induction furnace based vacuum magnesium production system and magnesium production method thereof |
| CN109797296A (en) * | 2017-11-17 | 2019-05-24 | 狄保法 | A kind of melt carbothermy magnesium smelting device |
| CN108746560A (en) * | 2018-08-14 | 2018-11-06 | 广州德志金属制品有限公司 | A kind of magnesium stove processing unit (plant) |
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| WO2021121312A1 (en) * | 2019-12-17 | 2021-06-24 | 郑州大学 | Method for carbothermic smelting of magnesium and co-production of calcium carbide |
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| CN112609091A (en) * | 2020-12-28 | 2021-04-06 | 金先奎 | Method for smelting magnesium metal by carbothermic reduction |
| CN114737057A (en) * | 2022-03-24 | 2022-07-12 | 东北大学 | Method for preparing high vapor pressure metal by carbothermic reduction |
| CN114870568A (en) * | 2022-03-24 | 2022-08-09 | 东北大学 | Device for smelting active high-vapor-pressure metal by carbon thermal reduction and using method thereof |
| CN114870568B (en) * | 2022-03-24 | 2023-06-27 | 东北大学 | Device for carbothermic reduction smelting of active high vapor pressure metal and use method thereof |
| CN114737057B (en) * | 2022-03-24 | 2024-03-26 | 东北大学 | Method for preparing high vapor pressure metal by carbothermal reduction |
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| WO2018001265A1 (en) | 2018-01-04 |
| CN106011500A (en) | 2016-10-12 |
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