CN108298572A - The method and apparatus of ice crystal and carbon in waste slag of electrolytic aluminium is continuously detached using vacuum high temperature furnace - Google Patents
The method and apparatus of ice crystal and carbon in waste slag of electrolytic aluminium is continuously detached using vacuum high temperature furnace Download PDFInfo
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- CN108298572A CN108298572A CN201710355619.8A CN201710355619A CN108298572A CN 108298572 A CN108298572 A CN 108298572A CN 201710355619 A CN201710355619 A CN 201710355619A CN 108298572 A CN108298572 A CN 108298572A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
- C01F7/54—Double compounds containing both aluminium and alkali metals or alkaline-earth metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/18—Electrolytes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods continuously detaching ice crystal and carbon in waste slag of electrolytic aluminium using vacuum high temperature furnace, specifically include following steps：Waste slag of electrolytic aluminium is put into vacuum high temperature furnace, will be evacuated in stove, be then heated up to 10000C to 13000C, ice crystal distillation is detached with carbon, and then recycles ice crystal and carbon.The advantages that ice crystal and carbon in this method separation waste slag of electrolytic aluminium have generation temperature low, are swift in response, and the purity of obtained ice crystal is high, and production process is continuous, and production efficiency is high, and at low cost.Ice crystal in waste slag of electrolytic aluminium and carbon are detached, can be continuing with, pollution of the waste residue to ambient enviroment is reduced, and protect existing ice crystal resource, effect is greatly facilitated to sustainable development.Further include a kind of equipment for the above method, there is lower production cost, can effectively reduce utilization cost of the aluminum electrolysis industry to ice crystal and carbon, there is larger dissemination.
Description
Technical field
The present invention relates to a kind of continuously to be detached the method for ice crystal and carbon in waste slag of electrolytic aluminium using vacuum high temperature furnace and set
It is standby, belong to metal smelt technical field.
Background technology
It is by with the calcined coke and coal tar pitch of variable grain that metallic aluminium, which is with its anode of villiaumite-alumina eltrolysis method production,
It mixed for bonding agent, shake extrusion forming, then roasted and obtain through charing.It actually often produces one ton of aluminium and wants consumable anode charcoal
Block 470kg or so.And theoretical consumption only has 334kg.This has more 140kg than theory.The air being primarily due in electrolytic cell
The waste residue of loss and the carbon granules formation fallen down from anode with CO2 oxidizing anodes.Often produce one ton of aluminium to generate waste residue be 3 ~
5kg.It has seriously affected conductivity, and the viscosity of electrolyte, this is also required to worker and takes off out out of electrolytic cell, significantly affects big
Production efficiency.
The cathode and trough rim liner of cryolite-alumina fused-salt bath use carbonaceous material, typically with calcined coke,
Calcined anthracite or artificial graphite are primary raw material, and pitch bonding agent is added, and are roasted by 1000 ~ 1300 DEG C after kneading and compacting
It burns.And it is made firm by ramming between cathode and with carbon resistance rod paste between cathode and side wall, to prevent molten aluminum and electrolyte from electrolysis
Exudation in slot.In aluminium cell production process, small part sodium fluoride can also be reduced electrochemically as metallic sodium, whole in electrolytic cell
In a period, electrolyte and metallic sodium can be permeated into the carbonaceous material of cathode and trough side part liner always.Aluminium electrolytic cell cathode
General 4 ~ 6 years with the service life of trough side part liner.After electrolytic cell destroys, the cathode and trough side part liner of electrolyte have been permeated,
It is dug from electrolytic cell, and is stacked into specific place.Currently, there is no a technical and economically all feasible method will be positive
The method that pole, cathode and carbon in trough side part liner and electrolyte components are effectively separated recycling.
Method of the processing containing villiaumite electrolyte carbonaceous solids waste material is mainly the following at present：1）Floatation is such as
CN201521012259.4 and CN01138204.X is to carry out ball milling, floating breeze, anode scrap and with rear cathode carbon pieces together
Choosing, comprehensive utilization.Flotation one side product purity is inadequate, cannot be utilized effectively.On the other hand there are sewage and air pollution
Problem.2）Oxidizing roasting method such as patent of invention CN201610362643.X and 200410069389.1.It is recycling breeze and cathode
The method of fluoride salt in carbon block.Into breeze match a certain amount of aluminium oxide, by 550 ~ 930 DEG C burn-up charcoals, leave aluminium oxide and
Fluoride salt.It can return to electrolytic aluminium use.Recovery rate is relatively low in this way.All recycling are had adverse effect on.And it is molten with lye
Solution, and generate sewage.This leads to the problem of environment.3）High temperature evaporation method such as patent 201210512011.9 is by breeze through excessive
After choosing, it is burnt by 1700 DEG C.The villiaumites fusing point such as ice crystal or more is made up to, and villiaumite steam raising is caused to come out.It is this
Method benefit is charcoal and electrolyte to be completely separated out, is exactly that temperature is too high, causes cost too high, efficiency is too low.4）
Patent 201510269179.5 is that the side of charcoal and electrolyte components is separated and recovered in a kind of solid waste containing charcoal from aluminium molten-salt electrolysis
Method.The solid waste containing charcoal introduced in this method includes breeze, cathode carbon pieces and side wall brick fuel in aluminium cell.After these are used
Contain ice crystal, aluminum fluoride, sodium fluoride, calcirm-fluoride etc. in charcoal product.These are broken into 5 ~ 60mm with rear product, is less than 5mm
Part is 20 ~ 60mm particles by adding bonding agent batch mixing to be molded into size.These particulate materials are packed into vacuum tank, heating in vacuum
To 1000 ~ 1400 DEG C, it is allowed to fluoride and becomes gas evaporation to come out.To reach the target carbon granule and Fluoride Separation.
Under vacuum condition, villiaumite evaporating temperature is low, charcoal and villiaumite separation easy to implement.Therefore cost is relatively low, is a good method.But
It is that its particle size limitation is very tight, to be crushed processing for breeze, cathode carbon pieces and side wall carbon block and want batch mixing for thin
Processing and forming, this has adverse effect on dust and environmental pollution, and needs to take after reducing temperature after the completion of separation per stove
The production of next stove can just be carried out by going out the carbon of separation, and the discontinuity of production can not improve production efficiency, make mass energy in vain
Waste, is unfavorable for energy conservation and environmental protection.Moreover, the invention processing capacity is limited, it is to be improved.
In conclusion up to now with regard to known to the present invention, there has been no " continuously detach waste slag of electrolytic aluminium using vacuum high temperature furnace
The report of the method and apparatus of middle ice crystal and carbon ", to be guided out the purpose of the present invention.
Invention content
The purpose of the present invention is to provide a kind of ice crystal and carbon in waste slag of electrolytic aluminium are continuously detached using vacuum high temperature furnace
Method, ice crystal and carbon in continuous separation waste slag of electrolytic aluminium can be simple and efficient, and the ice crystal and carbon purity that recycle are higher.
A method of continuously detaching ice crystal in waste slag of electrolytic aluminium using vacuum high temperature furnace, step is：
Vacuum high temperature furnace debugging is normal, opens charging control valve, and part waste residue in feeding chamber is added in vacuum high temperature furnace, will be true
Empty stove is sealed, and opens vacuum extractor, which is evacuated to 20000 pas hereinafter, vacuum extractor with vacuum extractor
It runs well, and opens heating system, wait for that in-furnace temperature reaches 1000 DEG C or more, the ice crystal in waste residue starts distillation and taken out
Go out, the ice crystal gas of extraction is recycled since temperature reduction is frozen into particle, completes separation.
Feeding device is connected with vacuum extractor, after the charging of outside, will take out gas in feeding device, then by waste residue
Material is added in stove by several times, can continue to feed by feeding device after the completion of separation every time, without reducing in-furnace temperature, in this way may be used
Realize the continuity of charging.
Preferably, waste slag of electrolytic aluminium is fed by feeding device.
Preferably, after the completion of separation, remaining carbon is taken out by drawing mechanism from vacuum high temperature furnace.What is be continuously added to is useless
Slag carbon after separating at high temperature goes out ice crystal can be deposited on the lower part of vacuum high temperature furnace, and drawing mechanism takes out a part of carbon in stove,
Cooling system is disposed with around drawing mechanism, temperature can be taken out into air after being reduced to 400 DEG C or less, realize carbon
Continuous discharge.
Wherein, the mode of heating of vacuum high temperature furnace described in above equipment and method is that heating rod heating, induction coil add
Heat.
Wherein, the cooling of drawing mechanism described in above equipment and method uses water cooling, air cooling or natural cooling.
A kind of equipment continuously detaching ice crystal in waste slag of electrolytic aluminium using vacuum high temperature furnace, including high-temperature vacuum furnace, should
Vacuum high temperature furnace is heated by induction coil or heating rod, and is connected with vacuum extractor and ice crystal collector.It is described
It is equipped with feeding device above vacuum high temperature furnace, is equipped with drawing mechanism below, the feeding device includes that feeding chamber and charging are controlled
Valve processed, drawing mechanism include discharging bin, discharging control valve and cooling system.
Wherein, feeding chamber one end of feeding device is connected with high-temperature vacuum furnace interior, and is sealed by charging control valve
Connection, the feeding chamber other end can carry out external charging.
Wherein, feeding device is connect with vacuum extractor.
Wherein, discharging bin one end of drawing mechanism is connected with high-temperature vacuum furnace bottom, and is sealed by discharging control valve
Connection, the cooling system are set in discharging bin, which is additionally provided with material taking mouth.
Wherein, the thermocouple that temperature is measured and shown is equipped in cooling system.
Ice crystal and carbon in this method separation waste slag of electrolytic aluminium have generation temperature low, are swift in response, obtained ice crystal
Purity it is high, the advantages that production process is continuous, and production efficiency is high, and at low cost.Ice crystal in waste slag of electrolytic aluminium and carbon are carried out
Separation, can be continuing with, and pollution of the waste residue to ambient enviroment be reduced, and protect existing ice crystal resource, to sustainable development
Greatly facilitate effect.Lower production cost can effectively reduce utilization cost of the aluminum electrolysis industry to ice crystal and carbon, tool
There is larger dissemination.
The present invention detaches ice crystal using vacuum high temperature furnace, and feeding device exists with drawing mechanism in the present invention
The continuity of charging and discharging is realized in addition in system, without cooling, substantially reduces charging cooling during rolling and again every time
The duration of heating, improves work efficiency, and reduces energy consumption.According to the difference to feed every time, the guarantor under separation temperature can control
The warm time is different so that waste residue is fully detached.Continuously detached using vacuum high temperature furnace, can continuous processing waste residue amount it is big, and
Waste slag of electrolytic aluminium is not necessarily to crushing, reduces the requirement to waste residue material, improves work efficiency, reduces environmental pollution.Separation
Feeding device can continue after the completion plus waste material, drawing mechanism can take out the carbon in vacuum high temperature furnace, the oxidation of anti-blocking.
The speed of separating rate has direct relationship with temperature height, vacuum degree in stove.Temperature is higher, and air pressure is lower, point
It is faster from speed.
The ice crystal and carbon isolated are detected, separated ice crystal purity is more than 97%, and carbon purity is more than 98%.
It can thus be seen that separation method products therefrom purity using the present invention is far above the separating effect of other methods.To separation
The substance gone out is detected.
The concrete content table of comparisons is with reference to as follows.
| AlF3 | NaF | Al2O3 | C | |
| The carbon of collection | / | / | 0.5 | 98.6 |
| The ice crystal of separation | 48.8 | 58.9 | 0.2 |
Description of the drawings
Fig. 1 is ice crystal in continuous separation waste slag of electrolytic aluminium provided by the invention and the equipment used in carbon.
Specific implementation mode
The present invention will be further elaborated with the following Examples.
Referring to Fig.1, a kind of equipment continuously detaching ice crystal in waste slag of electrolytic aluminium using vacuum high temperature furnace, including vacuum height
Warm stove 1, which is connected with vacuum extractor 5 and ice crystal collector 4 by induction coil 6, i.e., cold
Condenser.It is equipped with feeding device 2 above vacuum high temperature furnace 1, is equipped with drawing mechanism 3 below, feeding device 2 includes feeding chamber and adds
Expect control valve, feeding chamber one end of feeding device 2 is connected with 1 inside of vacuum high temperature furnace, and seals and connect by charging control valve
It connects, the feeding chamber other end can carry out external charging.Feeding device 2 is connect with vacuum extractor 5.Drawing mechanism 3 include discharging bin,
Discharging control valve and cooling system.The thermocouple that temperature is measured and shown is equipped in cooling system.Discharging bin one end and high temperature
1 bottom of vacuum drying oven is connected, and is tightly connected by discharging control valve, and the cooling system is set in discharging bin, the discharging
Storehouse is additionally provided with material taking mouth.
Embodiment 1
1, feeding chamber is added in waste slag of electrolytic aluminium, it is primary to be added 100 kilograms.
2, vacuum high temperature furnace debugging is normal, opens charging control valve and the waste residue in feeding chamber is added in vacuum high temperature furnace,
Vacuum extractor is opened, air pressure reaches 20000 pas, proceeds by sensing heating, and temperature rises to 1150 DEG C, and ice crystal is vaporized by taking out
Vacuum plant is extracted out, is cooled and solidified by ice crystal collector and is recycled at particle, as ice crystal.
3,1150 DEG C of heat preservations, separation terminates, and takes out from vacuum high temperature furnace carbon by discharging bin, is then continued by feeding chamber
Waste residue is added.Be provided with water-cooling system in drawing mechanism, cooled down carbon with water cooling, wait for thermocouple displays temperature to 400 DEG C with
When lower, it is discharged by the material taking mouth of discharging bin.
4, through to its purity of ice crystal chemical analysis, up to 97.3%, carbon purity 98.3% can be reused effectively and is being electrolysed
In aluminium.
Embodiment 2
1, feeding chamber is added in waste slag of electrolytic aluminium, it is primary to be added 150 kilograms.
2, vacuum high temperature furnace debugging is normal, opens control valve and the waste residue in feeding chamber is added in vacuum high temperature furnace, open
Vacuum extractor, air pressure reach 10000 pas, proceed by sensing heating, and temperature rises to 1000 DEG C, and ice crystal is vaporized by vacuumizing
Device is extracted out, is cooled and solidified by ice crystal collector and is recycled at particle, as ice crystal.
3,1000 DEG C of heat preservations terminate to separation, are taken out from vacuum high temperature furnace carbon by discharging bin, then by feeding chamber after
It is continuous that waste residue is added.It is provided with water-cooling system in drawing mechanism, is cooled down carbon with the mode of water cooling, waits for thermocouple displays temperature extremely
At 400 DEG C or less, it is discharged by the material taking mouth of discharging bin.
4, through to its purity of ice crystal chemical analysis, up to 97.1%, carbon purity 98.6% can be reused effectively and is being electrolysed
In aluminium.
Foregoing description has illustrated illustrating and describing for invention.It is not configured to limit the invention to disclosed
Form and mode.According to above mode, it can be changed or be changed accordingly.Discuss that example is to be better described
The principle of the present invention and the practicality, to be carry out various modifications using the present invention and meet other specific demands.It is all this
A little modifications and variations are understood when according to fair and legal right, and according to accessory claim, these modifications and variations are all
It is within the scope of the present invention.
Claims (8)
1. a kind of method continuously detaching ice crystal in waste slag of electrolytic aluminium using vacuum high temperature furnace, step are：By electrolytic aluminium waste
Slag is put into vacuum high temperature furnace, which is evacuated to 20000 pas hereinafter, temperature is increased to 1000 with vacuum extractor0C is extremely
13000C heats waste slag of electrolytic aluminium in the state of vacuum, ice crystal is made to be detached with carbon, and ice crystal distils and by vacuumizing
Device is pumped into collection device and is collected, and residue is carbon.
2. the method for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 1,
It is characterized in that：Waste slag of electrolytic aluminium is fed by feeding device, and after the completion of separation, remaining carbon is by drawing mechanism from high temperature
It is taken out in vacuum drying oven.
3. the method for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 2,
It is characterized in that：After the completion of separation, it can continue to add waste material by the feeding device.
4. the method for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 1,
It is characterized in that：The mode of heating of the vacuum high temperature furnace is heating rod heating, induction coil heating.
5. the method for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 2,
It is characterized in that：Carbon after the separation cooling down in drawing mechanism is passed through air trapping to 400 DEG C or less again.
6. the method for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 5,
It is characterized in that：The cooling of the drawing mechanism uses water cooling, air cooling or natural cooling.
7. a kind of equipment continuously detaching ice crystal in waste slag of electrolytic aluminium using vacuum high temperature furnace, it is characterised in that：Including vacuum
High temperature furnace, the high-temperature vacuum furnace are connected with vacuum extractor and ice crystal collector；And it is equipped with and adds above vacuum high temperature furnace
Expect device, be equipped with drawing mechanism below, the feeding device includes feeding chamber and charging control valve, and drawing mechanism includes discharging
Storehouse, discharging control valve and cooling system.
8. the equipment for utilizing vacuum high temperature furnace continuously to detach ice crystal and carbon in waste slag of electrolytic aluminium according to claim 7,
It is characterized in that：The feeding device is connect with vacuum extractor.
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| CN201710355619.8A CN108298572A (en) | 2017-05-19 | 2017-05-19 | The method and apparatus of ice crystal and carbon in waste slag of electrolytic aluminium is continuously detached using vacuum high temperature furnace |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894600A (en) * | 2015-05-25 | 2015-09-09 | 东北大学 | Method for separating and recovering carbon and electrolytic constituents from aluminum molten salt electrolysis carbon-containing solid wastes |
| CN105648216A (en) * | 2016-01-12 | 2016-06-08 | 昆明理工大学 | Continuous vacuum distillation device for solid feeding and discharging and application method of device |
| CN106238439A (en) * | 2016-08-16 | 2016-12-21 | 红河学院 | The method of aluminium electrolytic tank vacuum distilling defluorinate |
| CN106433850A (en) * | 2016-09-21 | 2017-02-22 | 红河学院 | Method for preparing cement kiln fuel from aluminium electrolysis waste cathodes |
-
2017
- 2017-05-19 CN CN201710355619.8A patent/CN108298572A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894600A (en) * | 2015-05-25 | 2015-09-09 | 东北大学 | Method for separating and recovering carbon and electrolytic constituents from aluminum molten salt electrolysis carbon-containing solid wastes |
| CN105648216A (en) * | 2016-01-12 | 2016-06-08 | 昆明理工大学 | Continuous vacuum distillation device for solid feeding and discharging and application method of device |
| CN106238439A (en) * | 2016-08-16 | 2016-12-21 | 红河学院 | The method of aluminium electrolytic tank vacuum distilling defluorinate |
| CN106433850A (en) * | 2016-09-21 | 2017-02-22 | 红河学院 | Method for preparing cement kiln fuel from aluminium electrolysis waste cathodes |
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