CN104894382B - Recovery treatment method of electrolytic aluminum ash and refractory material lining waste - Google Patents
Recovery treatment method of electrolytic aluminum ash and refractory material lining waste Download PDFInfo
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- CN104894382B CN104894382B CN201510296489.6A CN201510296489A CN104894382B CN 104894382 B CN104894382 B CN 104894382B CN 201510296489 A CN201510296489 A CN 201510296489A CN 104894382 B CN104894382 B CN 104894382B
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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
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Abstract
The invention discloses a recovery treatment method of electrolytic aluminum ash and a refractory material lining waste; the refractory lining waste is divided into an impermeable insulation waste and a silicon carbide waste; and the method comprises the following steps: (1) the impermeable insulation waste is crushed and levigated to mix with the aluminum ash to press a pellet; (2) vacuum distillation: electrolyte and metal sodium are crystallized on a crystallizer; the remainder part has main components of Al2O3 and SiO2; the silicon carbide waste is distilled at a temperature of 1000-1200 DEG C in vacuum after being crushed; the electrolyte is crystallized on the crystallizer; and the remainder part is a silicon nitride and silicon carbide refractory material. The method is simple in flow; the useful components can be fully recycled; the recovery cost is low; and meanwhile, the environmental pollution is reduced, so that the application prospect is excellent.
Description
Technical field
The present invention relates to a kind of recovery and treatment method of electrolytic aluminum scraps, more particularly to a kind of electrolytic aluminium aluminium ash and fire proofed wood
Expect the recovery and treatment method of liner waste material.
Background technology
Aluminium is the metal material for being only second to steel, and its yield is first of non-ferrous metal.The production capacity of Chinese aluminium electroloysis in 2014
It it is 35,840,000 tons, actual production is 28,100,000 tons, is the first in the world Chan Lv big countries.
Aluminum electrolysis discharge four kinds of solid wastes, and two of which is useless charcoal cathode inner lining and anode breeze, belongs to main
It is charcoal and the solid waste of electrolyte components to want composition, has introduction in the patent application of Application No. 2015102691795.
In two kinds of other waste materials, the first is aluminium ash：Aluminium ash is the aluminium slag of pouring aluminium ladle adhesion, holding furnace slag hitting generation
Aluminium slag and aluminum casting during produce aluminium slag is screened or ball milling after again after the aluminium slag of the screened reunion shape for extracting bulk
Obtained from the lower grey powder-material of sieve；The main component of aluminium ash is aluminum oxide, and it also contains portion in addition to containing a small amount of aluminium carbide
Divide fine aluminium powder, it contains the 10-15% that metal aluminum amount accounts for aluminium ash total amount；Aluminium ash in aluminum oxide due to density it is small, be not suitable for
As the raw material of aluminium electroloysis, other purposes are not found still at present, therefore the individual workship of electrolytic aluminium factory or treatment aluminium slag is general
All this aluminium ash is landfilled as waste material or it is abandoned, this not only causes the waste of resource, and causes shadow to environment
Ring.
The refractory lining waste material that also a kind of solid waste is produced when being electrolytic cell overhaul, this refractory lining
A waste material part is that the infiltration of cathode carbon pieces bottom and sidepiece has electrolyte and alkali metal, is produced with electrolyte and metallic sodium reaction
The Impervious Materials and flame-proof thermal insulation material waste material of the compound being made up of alkali metal oxide, aluminum oxide and silica；Another portion
Point it is that the infiltration of trough side part has electrolyte and metallic aluminium and the carbonization by silicon nitride bonded silicon corroded by electrolyte and metallic aluminium
Silicon fire resistive material liner waste material；Only used on the electrolytic cell of larger current intensity by the silicon carbide lining of silicon nitride bonded silicon, this
Two parts are referred to as the refractory lining waste material of electrolytic cell.
At present in electrolytic cell overhaul, both the waste refractory materials liners dug from electrolytic cell are not all recycled
And treatment, but open area is deposited in, surrounding environment is impacted.
The content of the invention
The refractory lining waste material produced during for current electrolysis aluminium manufacturer to aluminium ash and electrolytic cell overhaul is not yet had
Effect is reclaimed and utilized, and the problem impacted to environment, and the present invention provides a kind of electrolytic aluminium aluminium ash and refractory lining gives up
The recovery and treatment method of material.
Refractory lining waste material of the invention is divided into two parts, and Part I is Impervious Materials and flame-proof thermal insulation material waste material,
Referred to as anti-seepage heat preservation waste material；Part II is that, by the Tercod liner waste material of silicon nitride bonded silicon, referred to as carborundum gives up
Material.
Anti-seepage heat preservation waste recovery processing method of the present invention is crushed anti-seepage heat preservation waste material and after grinds, mixed with aluminium ash
Combined pressure is made group, then under vacuum and 1000 ~ 1400 DEG C of temperature conditionss, using the aluminium in aluminium ash by anti-seepage heat preservation waste material
Oxidation sodium reduction generation metallic sodium, while by the electrolyte components Distillation recovery in anti-seepage heat preservation waste material, making electrolyte components
With sodium oxide molybdena Component seperation, harmless treatment is realized.
In above-mentioned anti-seepage heat preservation waste material can contain a small amount of alfer, be due to leak into damaged groove the aluminium liquid of bottom land with
Cathode steel bar reaction generation, the aluminium in alfer also assists in redox reaction.
Anti-seepage heat preservation waste recovery processing method of the invention is carried out according to the following steps：
1st, by anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixing ratio
Example is 1 by weight:（0.5~2）, it is re-compacted into pelletizing；
2nd, pelletizing is placed under the conditions of vacuum≤100Pa, 1000 ~ 1400 DEG C of vacuum distillations is heated to, during vacuum distillation
Between be 1 ~ 10h, electrolyte and metallic sodium crystallize on crystallizer, and the main component of remainder is Al2O3And SiO2。
The reaction equation of the above method is：
3Na2O+2Al(l)→6Na+ Al2O3(s) （1）
With
CaF2(s)→CaF2(g) （2）；
Wherein react（1）Occur at 800 ~ 1100 DEG C, when having CaF in anti-seepage heat preservation waste material2When, reaction（2）Occur, occur
Temperature is at 1300 ~ 1400 DEG C.
In the above method, when anti-seepage heat preservation waste material contains KF and/or LiF, KF and/or LiF is crystallized on crystallizer, when
K2O and/or Li2During O, what is crystallized on crystallizer also has K and/or Li, and the reaction equation of step 2 also includes：
LiF(s) →LiF(g) （3）、
KF(s) →KF(g) （4）、
3K2O(s) +2Al(l)→6K(g)+Al2O3(s) （5）
And/or
3Li2O(s) +2Al(l)→6Li (g)+Al2O3(s) （6）；
Wherein react（3）With（4）Occur at 800 ~ 1100 DEG C.
Above-mentioned electrolyte main component is ice crystal and sodium fluoride, also containing aluminum fluoride and magnesium fluoride, can also be contained
Calcirm-fluoride, potassium fluoride and lithium fluoride；There are metallic potassium and/or gold when also being collected containing potassium fluoride and/or during lithium fluoride, in crystallizer
Category lithium.
Above-mentioned remainder is used as the raw material for producing new Impervious Materials.
Silicon carbide waste recovery and treatment method of the invention is that silicon carbide waste is placed in vacuum tank, 1000 ~ 1200
It is evaporated in vacuo at a temperature of DEG C, using the spy of the very high-vapor-pressure of the electrolysis of fluorides matter being etched into silicon carbide waste
Property, by electrolyte and carborundum Component seperation.
Silicon carbide waste recovery and treatment method of the invention is：
Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material.
Above-mentioned silicon nitride combined with silicon carbide refractory material as the silicon carbide brick for producing new silicon nitride bonded silicon raw material
In the above method, the pressure for being pressed into pelletizing is 30 ~ 100MPa.
Method of the present invention flow is simple, and useful constituent can be recycled fully, and cost recovery is low, while it is dirty to reduce environment
Dye, has a good application prospect.
Brief description of the drawings
Fig. 1 is that the electrolytic aluminium aluminium ash in the embodiment of the present invention shows with the recovery and treatment method flow of refractory lining waste material
It is intended to.
Specific embodiment
The composition of the anti-seepage heat preservation waste material in the embodiment of the present invention contains Al by weight percentage2O310 ~ 60%, F 2 ~ 10%,
Ca 1 ~ 10%, Na 2 ~ 20%, SiO210 ~ 60%, remaining is impurity.
Aluminium ash composition contains Al 10 ~ 30%, Al by weight percentage in the embodiment of the present invention2O330 ~ 60%, remaining is miscellaneous
Matter.
Pelletizing is pressed into the embodiment of the present invention for cylindric, diameter in 20 ~ 30mm, highly in 30 ~ 40mm.
The rate of recovery of electrolyte is more than 95% in the embodiment of the present invention.
Impurity weight content≤2% of silicon nitride combined with silicon carbide refractory material in the embodiment of the present invention.
Embodiment 1
By anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixed proportion
By weight it is 1:（0.5~2）, it is re-compacted into pelletizing；The pressure for being pressed into pelletizing is 30 ~ 100MPa；
Pelletizing is placed under the conditions of vacuum≤100Pa, 1000 ~ 1400 DEG C of vacuum distillations are heated to, the time is evaporated in vacuo
It is 1 ~ 10h, electrolyte and metallic sodium are crystallized on crystallizer, the main component of remainder is Al2O3And SiO2, as production
The raw material of new Impervious Materials；
Electrolyte main component is ice crystal and sodium fluoride, also contains aluminum fluoride, magnesium fluoride, calcirm-fluoride, potassium fluoride and fluorine
Change lithium；
Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material, as the raw material of the silicon carbide brick for producing new silicon nitride bonded silicon.
Embodiment 2
By anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixed proportion
By weight it is 1:（0.5~2）, it is re-compacted into pelletizing；The pressure for being pressed into pelletizing is 30 ~ 100MPa；
Pelletizing is placed under the conditions of vacuum≤100Pa, 1000 ~ 1400 DEG C of vacuum distillations are heated to, the time is evaporated in vacuo
It is 1 ~ 10h, electrolyte and metallic sodium are crystallized on crystallizer, the main component of remainder is Al2O3And SiO2, as production
The raw material of new Impervious Materials；
Electrolyte main component is ice crystal and sodium fluoride；
Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material, as the raw material of the silicon carbide brick for producing new silicon nitride bonded silicon.
Embodiment 3
By anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixed proportion
By weight it is 1:（0.5~2）, it is re-compacted into pelletizing；The pressure for being pressed into pelletizing is 30 ~ 100MPa；
Pelletizing is placed under the conditions of vacuum≤100Pa, 1000 ~ 1400 DEG C of vacuum distillations are heated to（Anti-seepage heat preservation waste material
In have CaF2）, the vacuum distillation time is 1 ~ 10h, and electrolyte and metallic sodium are crystallized on crystallizer, the main component of remainder
It is Al2O3And SiO2, as the raw material for producing new Impervious Materials；
Electrolyte main component is ice crystal and sodium fluoride；
Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material, as the raw material of the silicon carbide brick for producing new silicon nitride bonded silicon.
Embodiment 4
By anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixed proportion
By weight it is 1:（0.5~2）, it is re-compacted into pelletizing；The pressure for being pressed into pelletizing is 30 ~ 100MPa；
Pelletizing is placed under the conditions of vacuum≤100Pa, 1000 ~ 1400 DEG C of vacuum distillations are heated to（Anti-seepage heat preservation waste material
In have CaF2）, the vacuum distillation time is 1 ~ 10h, and electrolyte and metallic sodium are crystallized on crystallizer, the main component of remainder
It is Al2O3And SiO2, as the raw material for producing new Impervious Materials；
Electrolyte main component is ice crystal and sodium fluoride；
Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material, as the raw material of the silicon carbide brick for producing new silicon nitride bonded silicon.
Claims (2)
1. the recovery and treatment method of a kind of electrolytic aluminium aluminium ash and refractory lining waste material, described refractory lining waste material point
It is two parts, Part I is Impervious Materials and flame-proof thermal insulation material waste material, referred to as anti-seepage heat preservation waste material；Part II is by nitrogenizing
The Tercod liner waste material that silicon is combined, referred to as silicon carbide waste；It is characterized in that carrying out according to the following steps：
（1）By anti-seepage heat preservation waste material crush and it is levigate to granularity below 80 mesh, then with aluminium ash be well mixed, mixed proportion is pressed
Weight ratio is 1:（0.5~2）, it is re-compacted into pelletizing；The composition of described anti-seepage heat preservation waste material contains Al by weight percentage2O3 10~
60%, F 2 ~ 10%, Ca 1 ~ 10%, Na 2 ~ 20%, SiO210 ~ 60%, remaining is impurity；Described aluminium ash composition by weight hundred
Divide than containing Al 10 ~ 30%, Al2O330 ~ 60%, remaining is impurity；
（2）Pelletizing is placed under the conditions of vacuum≤100Pa, 1300 ~ 1400 DEG C of vacuum distillations are heated to, the vacuum distillation time is
1 ~ 10h, electrolyte and metallic sodium are crystallized on crystallizer, and the main component of remainder is Al2O3And SiO2；
（3）Silicon carbide waste is crushed to granularity in below 60mm, is subsequently placed under the conditions of vacuum≤100Pa, be heated to
1000 ~ 1200 DEG C, 1 ~ 10h is evaporated in vacuo at 1000 ~ 1200 DEG C, electrolyte is crystallized on crystallizer, and remainder is silicon nitride
Carborundum refractory material.
2. the recovery and treatment method of a kind of electrolytic aluminium aluminium ash according to claim 1 and refractory lining waste material, it is special
Levy is that the described pressure for being pressed into pelletizing is 30 ~ 100MPa.
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| CN107352567B (en) * | 2016-05-09 | 2019-10-18 | 青海大学 | The method that vacuum reduction distilation prepares high purity aluminium oxide |
| CN106517209A (en) * | 2016-11-07 | 2017-03-22 | 中国铝业股份有限公司 | Method for treating spent cathodes of spent potlinings of aluminum electrolysis cells |
| CN106744964B (en) * | 2016-11-21 | 2018-08-24 | 西北矿冶研究院 | Process for recovering silicon carbide from silicon carbide waste |
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| CN108275684B (en) * | 2017-05-19 | 2022-07-26 | 上海彭浦特种耐火材料厂有限公司 | Method for recycling waste silicon nitride combined silicon carbide brick produced by aluminum electrolytic cell |
| CN108585826B (en) * | 2018-05-17 | 2021-03-02 | 东北大学 | Method for preparing magnesium aluminate spinel by using secondary aluminum ash |
| CN109207738B (en) * | 2018-11-30 | 2020-07-10 | 东北大学 | Treatment method of waste refractory material of aluminum electrolytic cell |
| CN110144457B (en) * | 2019-05-15 | 2020-09-15 | 东北大学 | Method for preparing aluminum-silicon-iron alloy by carbon thermal reduction of aluminum ash pretreatment |
| CN110016557B (en) * | 2019-05-15 | 2020-05-12 | 东北大学 | Method for preparing ferro-silicon-aluminum by smelting aluminum ash serving as raw material in electric arc furnace |
| CN111499397B (en) * | 2020-04-15 | 2021-04-09 | 中南大学 | Method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues |
| CN113277517B (en) * | 2021-05-24 | 2022-06-03 | 昆明理工大学 | Method for separating electrolyte in waste cathode carbon block of aluminum electrolysis and synchronously producing metal silicon |
| CN115124357B (en) * | 2022-05-12 | 2023-03-21 | 郑州大学 | Method for preparing dry type impermeable material by using aluminum ash clinker |
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