• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    In a method of reclaiming spent carbonaceous cathode material, particularly spent aluminum production cathode trays, wherein the cathode material is fed to a shaft furnace and contained in the shaft furnace for gasification of carbon at thermal treatment temperatures above the ignition temperature of carbon and above the vaporization temperature of the consumed cathode material The reaction gases are passed in a first longitudinal section of the shaft furnace in co-current with the carbon and in a second longitudinal section of the shaft furnace in countercurrent to the carbon, wherein the reaction gases withdrawn from a region of the shaft furnace with an enlarged cross-section between said longitudinal sections and subjected to a post-treatment become.
    公开号:AT510686A4
    申请号:T245/2011
    申请日:2011-02-23
    公开日:2012-06-15
    发明作者:Alfred Dipl Ing Edlinger；Johann Dr Daimer
    申请人:Sgl Carbon Se；
    IPC主号:
    专利说明:

    • ft ····· ft Μ ··································································································· i - .............
    The invention relates to a method for processing spent carbonaceous cathode material, in particular spent cathode tubs from aluminum production, in which the cathode material fed to a shaft furnace 5 and in the shaft furnace for the gasification of carbon a thermal treatment at temperatures above the ignition temperature of the carbon and above the evaporation temperature of subjected in the spent cathode material contained toxins. 10
    In aluminum production according to the Hall-Heroult process, the reduction of aluminum oxide takes place in the melt-flow selektrolyse. The electrolysis cell usually consists of a steel tub, which is lined with carbon material {graphite / anthracite) 15. The carbon lining serves as a cathode in the electrolysis and is therefore referred to as a cathode trough in the sequence. Spent potliners, also called Spent Potliners, are produced in large quantities in aluminum production using the Hall-Heroult process and have always been a disposal problem due to their high levels of toxins. The toxins are especially cyanide formed from the carbon of the cathode pans and the nitrogen of the air, and various metal fluorides, such as sodium and aluminum fluoride, which are formed from the metal species contained in the bauxite together with the fluoride of the cryolite used in the Hall-Heroult process. When exchanging the used cathode tubs, they are removed from the electrolysis cell together with a refractory casing, so that the Spent Potliner additionally contains aluminum, silicon and magnesium oxide from the refractory material. 30 • t * f »« · · · · «· Ml • * * · ·» v «Φ φ - 2 - .............
    A method as mentioned above has been known, for example, from Canadian patent application CA 2 308 545 A1.
    In this process, spent cathode tubs from aluminum production are gasified in a shaft furnace and the reaction gases formed are withdrawn. A disadvantage of the procedure according to this prior art, however, that the alkalis also contained in the spent cathode tubs tend in such shaft furnaces to form circuits and therefore in the shaft furnace anrei-10 brazen and approaches and hanging phenomena and increased refractory wear and dust discharge and lead to a reduced quality of possibly formed slag from the starting materials. It is therefore an object of the present invention to provide an improved method with which said toxins can be completely separated and recovered from the spent cathode material and at the same time the formation of alkali cycles is suppressed. 20
    To achieve this object, the method mentioned above according to the invention further developed such that the reaction gases in a first longitudinal section of the shaft furnace in cocurrent with the carbon and in a two-th th longitudinal section of the shaft furnace are conducted in countercurrent to the carbon and that the reaction gases from one area the shaft furnace with an enlarged cross-section, in particular enlarged diameter, deducted between said longitudinal sections and a subsequent treatment be tered. The fact that the reaction gases are withdrawn in a central region along the longitudinal axis of the shaft furnace (middle gas vent), alkali cycles are interrupted and the reaction gases, the said poison- ·· ♦ · · · · ···· # · · · · · · · * Ft "ft. Ft. Ft." "Ft." "
    Substances in the form of sodium fluoride (NaF), hydrofluoric acid (HF), nitrogen (N2) and possibly other alkali metal and alkaline earth metal fluorides in addition to synthesis gas (CO + H2) contained, can be fed to a further workup. 5
    By itself, the process is autothermic due to the high C content when the carbon has reached the ignition temperature and sufficient oxygen is available for gasification. In order to start the process or support it during the process, however, it is provided according to a preferred embodiment that energy for the thermal treatment is introduced by electrical induction into the carbon to be worked up. In this case, in the region of the feed end of the shaft furnace, induction coils are arranged around the circumference of the shaft furnace, with which an induction field is built up, to which the introduced carbon of the used cathode material couples and thereby heats up. As an alternative to this induction method, it would be conceivable to give up a subset of already glowing coke or graphite, whereby the carbon of the consumed cathode material can likewise be brought to reaction temperature.
    The shaft furnace or its longitudinal sections can in this case have a circular cross section. However, if the shaft furnace is inductively heated, a rectangular section embodiment is preferred. This in particular due to the skin effect, which leads to the fact that the penetration depth of the electrodynamic field is limited. 30
    In order to maintain the carbonization of the carbon, it is provided according to a preferred embodiment of the present invention that in the first and / or second or fifth case, the first and / or second In the longitudinal section of the shaft furnace, oxygen is blown into the shaft section of the shaft furnace. In the areas in which the oxygen encounters the at least ignition temperature heated carbon, an oxidation of the carbon takes place to CO2, which, however, is again reduced to CO in the carbon bed in the shaft furnace after the Boudouard equilibrium. Thus, there is no complete combustion, but only a gasification of the carbon, whereby calorific value-containing carbon monoxide can be obtained. The cyanide (CN) contained in the spent cathode material in Figure 10 is also converted to carbon monoxide and nitrogen under the prevailing reaction conditions and thus completely destroyed. For the separation of alkalis and fluoride, the process according to the invention is preferably further developed in such a way that water or water vapor is injected in the first and / or second longitudinal section of the shaft furnace. Fluorides and alkalis, which are present for example as sodium fluoride, 20 are volatilized in the presence of water or water vapor according to the following reaction scheme and thereby converted into the gas phase:
    2NaF + H20- > Na 2 O + 2HF 25 Na 2 O + C-2Na 4 CO
    Na20 4 CO -► 2Na 4 C02
    The elemental sodium is gaseous and is removed via the center gas vent before circuits form in the shaft furnace 30. In the gas phase, in which hydrofluoric acid (HF) is included, sodium fluoride is formed again and can be deposited in the subsequent exhaust gas treatment. ··· «··· • 9 ·« · · · φ «· • ♦ · · # · | »· · · # ♦ ·· ♦ · ·« · · Φ · · · Φ «φ φ« - 5 - .............
    According to a preferred embodiment, the method according to the invention is carried out in such a way that oxygen and water or water vapor are blown into the shaft furnace with the aid of lances. This measure 5 addresses the problem that when oxygen or water or water vapor are blown in only via nozzles which open on the wall of the shaft furnace, only the edge zones of the shaft furnace or the carbon bed are fed in the shaft furnace, while the inner Area 10 of the cross section of the carbon bed remains underserved and in these areas, the reaction rate is therefore very low or an autothermal procedure may not even be achieved. By introducing oxygen and water or water vapor with the aid of lances, the substances mentioned can be introduced, for example, precisely at the points which lie in the region of the induction heating, whereby reaction spaces are generated which are sufficiently hot that the process subsequently running along the entire shaft furnace autotherm ab-20. At this point, powdered or dusty spent carbonaceous cathode material, in particular cathode pans can be blown.
    If the carbon of the spent cathode material in the shaft furnace is not completely gasified, the process may preferably be developed such that non-gasified carbon is dissolved in an iron bath. An iron bath ensures an outstanding solution kinetics for carbon and can be easily regenerated by blowing in oxygen, so called fresh. The injection of oxygen can also be carried out continuously to keep the iron bath constantly C-undersaturated. - 6 99 • 9 9 9 9 9 9 9 9 9 9 i * M • • 9 9 • · · · Φ · ΦΦ
    In the process of the present invention using an iron bath, a particularly advantageous effect may be achieved with respect to the work-up of spent cathode tubs containing refractory lining residues when, as in a preferred embodiment of the present invention, it consumes the spent carbonaceous cathode material the task on the shaft furnace Ca carrier for slagging of refractory material can be added. The Ca-carriers react with the aluminum, silicon and magnesium oxides of the refractory material to form a high-grade slag which has excellent hydraulic properties and can therefore be used advantageously in the cement industry for the production of hydraulic binders. As a Ca carrier 15, for example, CaO comes into question. CaO is available in the form of steel slag or burnt lime and can be added to the process as large as possible in order to keep the carbon bed or column thoroughly permeable. However, as an alternative to the process procedure just described using an iron bath, the process according to a preferred embodiment can also be developed in such a way that the carbon of the cathode material is completely gasified and the remaining cal-zinc is discharged. In this case, no Ca-carrier is added and there is a dry discharge of virtually carbon-free calcine consisting of aluminum and silica, which can also be found in the cement industry use.
    It has been observed that the calcinate may decompose into carbonaceous powder. Due to the powder form, however, this gas is no longer gas-permeable
    • • • • • ♦
    Sig and the corresponding shaft furnace part has no Durchgasbarkeit more. The following treatment options are conceivable. There may be a post-treatment on the iron bath as described above. Alternatively, the Pul-5 ver be treated for decarburization by means of steam, whereby a simultaneous cooling is achieved due to the endothermic heterogeneous water gas reaction.
    As already indicated above, elemental-10 res sodium and also sodium oxide (Na 2 O) recombine in the gas phase in the presence of hydrofluoric acid (HF) to sodium fluoride (NaF). For sodium oxide, the reaction equation should be given as follows: 15 Na20 + 2HF 2NaF + H20 For the gaseous sodium, the reaction equation should be given as follows: 20 Na + HF - > NaF + hH2
    The following side reaction can be observed: 2Na + H20 - ¥ Na20 + H2 25
    If problematic but economically interesting hydrofluoric acid is to be obtained in the gas phase, the process must be carried out with strongly acidic slag. In the presence of a strongly acidic slag, wherein the acidic component can be formed, for example, by silicon oxide and / or aluminum oxide, the formation of hydrofluoric acid takes place according to the following reaction equation: ## EQU1 ##
    • * «· · · * • ····« »« • ♦ · * · · · * · · · · · · · ·
    2NaF + SiO 2 + H 2 O - > Na 2 SiO 3 + 2HF or
    NaF + Al 2 O 3 + H 2 O NaAl 2 O 4 + HF 5 In order to control the products obtained in the gas phase, depending on the respective wishes, the method is preferably developed in such a way that the basicity in the shaft furnace by the addition of basic or acidic additives, in particular CaO or Si02, set to 10.
    A particularly preferred procedure provides that the addition of basic and acidic additives is carried out alternately. In this way, 15 sodium fluoride and hydrofluoric acid are alternately obtained. The hydrofluoric acid can be reacted with alumina (Al 2 O 3) to aluminum fluoride {AIF 3) and water, whereby the aluminum fluoride can be further processed with the sodium fluoride (NaF) obtained in the basic process to cryolite (Na 3 AlFe), which in turn in the aluminum production after the Hall Heroult process can be used. 12NaF + 4A1F3 4Na3AlF6 25 If the cargo of toxic substances such as cyanides, alkalis and their fluorides is too high, it may occur that the carbon of the spent cathode material is not coupled by electrical induction in the heating described above. In this case, the method may be preferably further developed such that unconsumed graphite or coke is added in addition to the carbon of the used cathode material. The unconsumed carbon couples at an appropriate frequency to the inductance. * * ♦ · φ · · · · · · · · · · · · · · · · · · · · _ eg_ ···· «· φφ φφ φ onsfeld and heats up, whereby the actual carbon to be worked up is also brought to temperature by the contact with the glowing graphite or coke. 5 Preferably, the process is carried out such that the reaction gases are withdrawn at temperatures of 800 ° C to 1200 ° C, in particular 900 ° C to 1100 ° C, in particular 1000 ° C and fed to the aftertreatment, whereby a condensation of the reaction gases or toxins is prevented in the line systems and a controlled exhaust gas treatment can be ensured.
    The invention will be explained in more detail below with reference to embodiments shown schematically in the drawing. 4 shows an overall view of the method according to the invention and FIGS. 5 and 6 show alternative embodiments of the shaft furnace for Durchftih-20 tion of the method according to the invention with particular attention to the discharge of the shaft furnace.
    In Fig. 1, 1 denotes a shaft furnace, which in the implementation of the method according to the invention at the 25 position 2 spent cathode tubs, which are also known as Spent Potliner, abandoned in broken form. The carbon pieces are moved by means of a rotary valve 3 in the shaft 4 of the shaft furnace 1, which can be introduced 5 5 oxygen at the height of the rotary valve 3 via a loop 30 line. Indicated by 6 are induction loops which introduce an induction field into the cross-section of the shaft furnace 1, so that the carbon of the spent cathode troughs is coupled to the shaft ························································································. ············································································································································································································································ is heated to 800PC. In the area 7 of the shaft furnace, the shaft has a larger diameter compared to the first axial longitudinal section 8 and the second axial longitudinal section 9, so that the reaction gases can be withdrawn from an annular space 10 as symbolized by the arrow 11. The reaction gases contain, as already described, carbon monoxide, sodium fluoride, sodium, nitrogen, hydrofluoric acid, hydrogen and optionally Be-10 rylliumfluorid as main components. Characterized in that the carbon of the spent cathode tubs is consumed by the gasification reaction, the present in the shaft furnace carbon column or bulk 12, which is yes 15 formed by the carbon of the spent cathode material, decreases in the direction of arrow 13 from. Characterized in that the reaction gases are withdrawn in the region 7 from the annular space 10, the reaction gases in the first longitudinal section 8 are guided in cocurrent with the carbon and in the second longitudinal section 9 of the shaft furnace in countercurrent to the carbon 20. In addition to the ring line 5 for the addition of oxygen and / or water or water vapor in the upper region of the shaft furnace further nozzles 14 are mounted in the second longitudinal section 9 of the shaft furnace through which also oxygen and / or water or water vapor can be blown 25. Other nozzles with the same functionality are located at position 15. With 16 is another rotary valve designated over which calcine can be discharged. While the upper part of the second longitudinal section 9, which has the nozzles 14, represents a Gegenstromheizstrecke, the lower portion 17 is to be understood as a cooling section, as above the nozzles 15, especially water in liquid
    Form and possibly introduced as steam or wet steam.
    An alternative to the process guide shown in FIG. 1 is shown in FIG. While in FIG. 1 a complete gasification of the carbon is to take place, non-gassed carbon can be dissolved in an iron bath 18 in the process control according to FIG. 2. Otherwise, the shaft furnace is constructed substantially the same and also has an extra area 7 with an enlarged diameter, from which the exhaust gases at the position 11 can be withdrawn. When the iron bath 18 is saturated with carbon, oxygen is injected into the iron bath via the lance 19, whereby at the position 20 pure carbon monoxide escapes, which can subsequently be thermally utilized. At position 21, fluoride-free slag can be tapped and sent for use in the cement industry. In the alternative embodiment of the shaft furnace according to FIG. 3, the iron bath 18 is arranged in the shaft furnace 1, wherein the Schlackenabstich of the fluoride-free slag takes place at the position 22. In area 23 of the shaft furnace there is a Abschmelzzone, in which there is a Eisenrekarburie-tion. As in the previous examples, the reaction gas is sucked out of an annular space 10 from the region 7 with an enlarged diameter at the position 11.
    In Fig. 4 it can be seen that in addition to the shaft furnace 1 ei-30 ne quenches 24, a soda lye absorber 25 and an aerosol demister 26 is part of the system for processing the spent cathode pans. The shaft furnace 1 has the features already described, in which case the extension is possible. ·································. ** · * ** ** * not carried over a rotary valve, but via a rotating cone 27, which is hollow and can be charged via the line 28, for example, with steam, so that the cone like a lance steam in the interior of the Carbon fill releases. The withdrawal of the reaction gases is again at the position 11, wherein the gases are passed in a first step in a gas cooler 29 before they get into the quenches 24. There they are mixed with water as aerosol and relaxed. Sodium 10 fluoride can be withdrawn at position 30. In the soda lye absorber 25, the neutralization of the hydrofluoric acid is carried out by sodium hydroxide solution. From the soda lye absorber 25, beryllium fluoride can be withdrawn at position 31. In the aerosol demister 26 residual sodium fluoride and 15 beryllium are separated from the gas stream, which is a pure synthesis gas consisting of carbon monoxide and hydrogen in the sequence.
    In Fig. 5 it can be seen that at the lower end 32 of the 20 shaft 4 of the shaft furnace 1, a lance 33 opens, which consists of an inner tube 34 and an outer tube 35. The two tubes 34 and 35 can be moved or telescoped against the shaft furnace and against each other, wherein for example by the inner tube of oxygen and by the outer tube water or water vapor is introduced into the shaft 4 of the shaft furnace 1. The fact that the lance 33 can be moved against the shaft, it is possible to mechanically manipulate the bed 12 in the shaft 4 of the shaft furnace 1, so that mechanical bridges ge-30 broken and the discharge in the area 36 is ensured. In region 36, a pivotable flap 37 is mounted, on which the calcinate comes to lie with the natural angle of repose .alpha..sub.a. When this angle of repose is reached * »* ······················································································· * If there is no further discharge of the calcine from the shaft 4, the flap 37 in this case is pivoted into the position 38 indicated by dashed lines so that the calcine falls into a discharge lock 39. Thereafter, the flap 37 is raised again to receive calcine again.
    The example of Figure 5 is further shown that the shaft furnace 1 in place of a circular cross-section 10 may generally also have a rectangular cross-section. This is illustrated in FIG. 5 by the dashed line 43, wherein both the first longitudinal section and the second longitudinal section may have a rectangular cross section at least in sections. As favorable here a clear width of 600 to 800 mm has been found. In order to realize the enlarged cross-section required for the middle gas take-off, the second longitudinal section of the shaft furnace has the wall 44 which is shown on the right in FIG. 5 and extends toward the exhaust opening.
    In Fig. 6, an alternative embodiment is shown, in which the calcine is conveyed by means of a Rüttelbodens 40 in the direction of a screw conveyor 41 to be supplied to 25 this way also a discharge lock 42. The Rüttelboden 40 in this case has a passage opening for a lance 33.
    权利要求:
    Claims (12)
    [1]
    • 4 · 4 ···································································································································································································································· A method of processing spent carbonaceous cathode material, in particular spent aluminum cathode tubes, in which the cathode material is fed to a shaft furnace and in the shaft furnace for gasification of carbon at temperatures above the ignition temperature of the carbon and above the evaporation temperature of 10 consumed cathode material is subjected to contained toxins, characterized in that the reaction gases in a first longitudinal section of the shaft furnace in co-current with the carbon and in a second longitudinal section of the shaft furnace in countercurrent to the carbon 15 are guided and that the reaction gases from a region of the shaft furnace with enlarged Cross section between said longitudinal sections deducted and subjected to a post-treatment.
    [2]
    2. The method according to claim 1, characterized in that energy is introduced for the thermal treatment by electrical induction in the carbon to be worked up.
    [3]
    3. The method according to claim 1 or 2, characterized in that in the first and / or second longitudinal section of the shaft furnace oxygen is blown.
    [4]
    4. The method of claim 1, 2 or 3, characterized gekenn-30 records that in the first and / or second longitudinal section of the shaft furnace water or water vapor is blown. [submitted


    [5]
    5. The method according to any one of claims 1 to 4, characterized in that oxygen and water or water vapor are injected by means of lances in the shaft furnace,
    [6]
    6. The method according to any one of claims 1 to 5, characterized in that non-gasified carbon is dissolved in an iron bath.
    [7]
    7. The method according to any one of claims 1 to 6, characterized in that the spent carbonaceous cathode material are added to the task on the shaft furnace Ca carrier for slagging of refractory material.
    [8]
    8. The method according to any one of claims 1 to 5, that the carbon of the cathode material completely gasified and the remaining calcine is discharged.
    [9]
    9. The method according to any one of claims 1 to 8, characterized 20 in that the basicity in the shaft furnace by the addition of basic or acidic additives, in particular CaO or SiO 2, is set.
    [10]
    10. The method according to claim 9, characterized in that the addition of basic and acidic additives is carried out alternately.
    [11]
    11. The method according to any one of claims 1 to 10, characterized in that in addition to the carbon of the cathode material needed 30 unspent graphite or coke is added. FOLLOW-UP • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ··· · ** »· # ·· ·
    [12]
    12. The method according to any one of claims 1 to 11, characterized in that the reaction gases are withdrawn at temperatures of 800 ° C to 1200 ° C, in particular 900 ° C to 1100 ° C, in particular 1000 ° C and fed to the aftertreatment wer-5 den , Vienna, 23 February 2011 Applicant by:

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    法律状态:
    2017-11-15| PC| Change of the owner|Owner name: SGL CFL CE GMBH, DE Effective date: 20171004 |
    2018-10-15| MM01| Lapse because of not paying annual fees|Effective date: 20180223 |
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    申请号 | 申请日 | 专利标题
    ATA245/2011A|AT510686B1|2011-02-23|2011-02-23|PROCESS FOR WORKING ON CONSUMED CARBOHYDRATED CATALOG MATERIAL|ATA245/2011A| AT510686B1|2011-02-23|2011-02-23|PROCESS FOR WORKING ON CONSUMED CARBOHYDRATED CATALOG MATERIAL|
    CN201280010277.1A| CN103415596B|2011-02-23|2012-02-22|To the used method being processed containing carbon cathode material|
    RU2013142926/05A| RU2556660C2|2011-02-23|2012-02-22|Method of processing of spent carbon containing material of cathode|
    UAA201311224A| UA105613C2|2011-02-23|2012-02-22|Method for processing used cathode material containing carbon|
    BR112013021512A| BR112013021512A2|2011-02-23|2012-02-22|method for processing carbon-containing cathode material|
    MYPI2013003052A| MY163997A|2011-02-23|2012-02-22|Method for processing used cathode material containing carbon|
    CA2827720A| CA2827720C|2011-02-23|2012-02-22|Method for processing used carbon-containing cathode material|
    PCT/EP2012/053006| WO2012113826A1|2011-02-23|2012-02-22|Method for processing used cathode material containing carbon|
    AU2012219652A| AU2012219652B2|2011-02-23|2012-02-22|Method for processing used cathode material containing carbon|
    EP12706807.0A| EP2678406B1|2011-02-23|2012-02-22|Method for processing used cathode material containing carbon|
    ES12706807.0T| ES2537286T3|2011-02-23|2012-02-22|Procedure for processing cathode material used with carbon content|
    ZA2013/06297A| ZA201306297B|2011-02-23|2013-08-21|Method for processing used cathode material containing carbon|
    US13/974,302| US9199109B2|2011-02-23|2013-08-23|Method for processing used carbon-containing cathode material|
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