SE202791C1 - - Google Patents
Info
- Publication number
- SE202791C1 SE202791C1 SE202791DA SE202791C1 SE 202791 C1 SE202791 C1 SE 202791C1 SE 202791D A SE202791D A SE 202791DA SE 202791 C1 SE202791 C1 SE 202791C1
- Authority
- SE
- Sweden
- Prior art keywords
- aluminum
- malt
- chamber
- salt
- gas
- Prior art date
Links
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 86
- 229910052782 aluminium Inorganic materials 0.000 claims description 65
- 150000003839 salts Chemical class 0.000 claims description 47
- GXCLVBGFBYZDAG-UHFFFAOYSA-N N-[2-(1H-indol-3-yl)ethyl]-N-methylprop-2-en-1-amine Chemical compound CN(CCC1=CNC2=C1C=CC=C2)CC=C GXCLVBGFBYZDAG-UHFFFAOYSA-N 0.000 claims description 46
- 238000001816 cooling Methods 0.000 claims description 25
- 239000000523 sample Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 238000005192 partition Methods 0.000 claims description 6
- 239000012809 cooling fluid Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 2
- 230000002485 urinary effect Effects 0.000 claims 2
- 229910000838 Al alloy Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 7
- 150000004820 halides Chemical class 0.000 description 6
- -1 aluminum halide Chemical class 0.000 description 5
- IZMHKHHRLNWLMK-UHFFFAOYSA-M chloridoaluminium Chemical compound Cl[Al] IZMHKHHRLNWLMK-UHFFFAOYSA-M 0.000 description 5
- 239000011833 salt mixture Substances 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011819 refractory material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- PQLAYKMGZDUDLQ-UHFFFAOYSA-K aluminium bromide Chemical compound Br[Al](Br)Br PQLAYKMGZDUDLQ-UHFFFAOYSA-K 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 208000018459 dissociative disease Diseases 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 241001289141 Babr Species 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- GPWHDDKQSYOYBF-UHFFFAOYSA-N ac1l2u0q Chemical compound Br[Br-]Br GPWHDDKQSYOYBF-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- NKQIMNKPSDEDMO-UHFFFAOYSA-L barium bromide Chemical compound [Br-].[Br-].[Ba+2] NKQIMNKPSDEDMO-UHFFFAOYSA-L 0.000 description 1
- 229910001620 barium bromide Inorganic materials 0.000 description 1
- WHGZNMDFTBSHJR-UHFFFAOYSA-M bromoalumane Chemical compound [AlH2]Br WHGZNMDFTBSHJR-UHFFFAOYSA-M 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PUGUQINMNYINPK-UHFFFAOYSA-N tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCN(C(=O)CCl)CC1 PUGUQINMNYINPK-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/0038—Obtaining aluminium by other processes
- C22B21/0046—Obtaining aluminium by other processes from aluminium halides
-
- 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
- C22B21/00—Obtaining aluminium
- C22B21/06—Obtaining aluminium refining
- C22B21/064—Obtaining aluminium refining using inert or reactive gases
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Description
KLASS INTERNATIONELLSVENSK C22 ba:21/06 PATENT- OCH REGISTRERINGSVERKET Ans. 7315/1958 inkom den 7/8 1958 utlagd den 21/6 196 ALUMINIUM LABORATORIES LTD, MONTREAL, CANADA satt att utvinna metalliskt aluminium ur aluminiumsubhalidgas jamte apparat harfor 17ppfinnare: A H Johnston och F W Southam Prioritet began! !ran den 9 august" 1957 (USA) Denna uppfinning hanfor sig till den sd kallade subhaliddestillation.en av aluminium, exempelvis ur metalliska material eller blandningar, vilka innehalla aluminium och andra metaller, och narmare bestamt hanfor sig denna uppfinning till utvinningen av metalliskt aluminium ur subhalidgasen eller -angan. I en sadan procedur, vilken i bland aven benamnes katalytisk destillation, behandlas del orena eller fororenade aluminiummaterialet for erhallande av en gasformig subhalid av aluminium vid forhajd temperatur, och gasen, som innehaller subhaliden, ledes till en kondensor, dar en omvand kemisk reaktion intraffar, innefattande dissociation av subhaliden under bildning av relativt ren aluminiuminetall tillsammans med normal aluminiumhalid, vilken at separerbar eller separeras, exempelvis foretradesvis forblir i gasform och ledes bort frau. kondensorn. Denna uppfinning avser att astadkomma en forbattrad apparat och ett forbattrat forfarande for utvinning av metalliskt aluminium, dvs. i smolt form, ur subhalidgasen genom den beskrivna dissociations- eller sonderdelningsreaktionen, och den for denna operation anvanda apparaten eller kondensorn kan betecknas sonderdelflings apparat. CLASS INTERNATIONAL SWEDISH C22 ba: 21/06 PATENT AND REGISTRATION AGENCY Ans. 7315/1958 was received on 7/8 1958 laid out on 21/6 196 ALUMINUM LABORATORIES LTD, MONTREAL, CANADA set to extract metallic aluminum from aluminum subhalide gas as well as apparatus for 17 inventors: A H Johnston and F W Southam Priority began! This invention relates to the so-called subhalide distillation of aluminum, for example from metallic materials or mixtures containing aluminum and other metals, and more particularly to this invention for the recovery of metallic aluminum. In such a procedure, which is sometimes referred to as catalytic distillation, the crude or contaminated aluminum material is sometimes treated to obtain a gaseous subhalide of aluminum at elevated temperature, and the gas containing the subhalide is passed to a condenser where a reverse chemical reaction occurs, comprising dissociating the subhalide to form relatively pure aluminum metal together with normal aluminum halide, which, when separable or separable, for example, preferably remains in gaseous form and is led away from the condenser. This invention aims to provide an improved apparatus and an improved procedure for recovery of meta llic aluminum, ie. in molten form, from the subhalide gas by the described dissociation or probe division reaction, and the apparatus or condenser used for this operation may be referred to as the probe division apparatus.
Enligt ett foredraget satt att genomfora subhaliddestillationsprocessen behan.dlas metallmaterialet i en lamplig konverter, i Aiken det upphettas och dar en halid i gasformigt tillsthnd bringas i kontakt med metallmaterialet. Haliden fir exempelvis aluminiumtriklorid eller -tribromid, dvs. AIG13 eller A1Br3, aven benamnda aluminiumklorid och aluminiumbromid. Vid lamplig temperatur, vanligen i omradet frail 1000° G och uppht, och under lampligt tryck, vilket kan vara atmosfarstryek eller under atmosfarstryck, reagerar den gasformiga haliden rued aluminiet i materialet under bildning av en gasformig aluminiumsubhalid, exempelvis en monohalid. Niir sa.- lunda behandlingsangan dr aluminiumtriklorid innehaller den frail konvertern avledda gasen atminstone en -vasentlig mangd aluminiummonoklorid. According to a preferred method of carrying out the subhalide distillation process, the metal material is treated in a suitable converter, in which it is heated and where a halide in gaseous state is brought into contact with the metal material. The halide fir, for example, aluminum trichloride or tribromide, i.e. AIG13 or A1Br3, also called aluminum chloride and aluminum bromide. At lamp temperature, usually in the range of 1000 ° C and above, and under lamp pressure, which may be atmospheric pressure or atmospheric pressure, the gaseous halide rued aluminum reacts in the material to form a gaseous aluminum subhalide, for example a monohalide. Thus, the treatment process in which aluminum trichloride contains the frail-derived gas at least a substantial amount of aluminum monochloride.
Den omvandlade gasen, vilken aven kan innehalla oreagerad halid, ledes till sonderdelningsomradet, dar en lamplig lagre temperatur uppratthalles, sh att den om-van.da reaktionen intrAffar, varvid subhaliden omvandlas tillbaka till aluminium och normal aluminiumhalid. Aluminiummetallen tillvaratages, medal' den gasformiga normala haliden ledes bort for utvinning och fOrnyad anvandning. Genom dessa kemiska operationer, vilka kunna benamnas subhaliddestillation, kan mycket rent eller relativt rent aluminium erhallas ur aluminiumhaltigt material med mycket lag-re renhet. The converted gas, which may also contain unreacted halide, is passed to the probe division area, where a suitable lower temperature is maintained, so that the converted reaction occurs, whereby the subhalide is converted back to aluminum and normal aluminum halide. The aluminum metal is recovered, and the gaseous normal halide is discarded for extraction and reuse. By these chemical operations, which can be called subhalide distillation, very pure or relatively pure aluminum can be obtained from aluminum-containing material with much lower purity.
Det har visat sig att sonderdelning av subhaliden och avsattnin.g av rent aluminium i small form effektivt kan astadkommas i en sonderdelningsapparat anordnad och fungerande som en kon.densor av s. k. stanktyp, dar gasen bringas i haftig kontakt med smalt aluminium, exempelvis genom att den ledes genom en mer eller mindre kontinuerlig stankning, strale eller dusch av den smalta metallen, sd att den forstorade ytan av den senare utovar den erforderliga kylverkan ph gasen for astadkommande av den omvanda eller sonderdelningsreaktionen i tillracklig grad. Operationen innefattar uppratthallandet av en avsevard massa av smalt aluminium (frail vilken 2201 791 stankningen eller duschen astadkommes) och kylningen av denna massa, dvs, avlagsnande av varme darifran sa att den for sonderdelningsreaktionen erforderliga temperaturen uppratthalles. I vanliga sadana kondensatorer for andra andamal astadkommes avlagsnande av varme medelst kylslingor, mantlar eller liknande, som genomgar den smalta metallen pi ett lampligt stalle, eller ibland anbragta i stankningsrummet Det har nu emellertid visat sig, att svarigheter uppsta vid den ovan beskrivna aluminiumsubhalidsonderdelningsoperationen, genom att de ror, sasom stalror, vilka ha tillracklig mekanisk styrka och tillracklig varmeledningsformaga, for att anvandas fOr kylmedlet, ha benagenhet att losas i small aluminium med atfoljande fororening av det senare. It has been found that probing of the subhalide and deposition of pure aluminum in small form can be effected efficiently in a probing apparatus arranged and functioning as a condenser of the so-called stench type, where the gas is brought into violent contact with narrow aluminum, for example by is passed through a more or less continuous stench, jet or shower of the molten metal, so that the enlarged surface of the latter exerts the required cooling action on the gas to bring about the converted or probing reaction to a sufficient degree. The operation involves maintaining a substantial mass of narrow aluminum (from which the stench or shower is effected) and cooling this mass, i.e., removing heat therefrom so that the temperature required for the probe division reaction is maintained. In ordinary such capacitors for other purposes, heat removal is effected by means of cooling coils, jackets or the like, which pass through the molten metal in a suitable stable, or sometimes placed in the stench chamber. that the tubes, such as stable tubes, which have sufficient mechanical strength and sufficient thermal conductivity, to be used for the coolant, have a tendency to loosen in small aluminum with consequent contamination of the latter.
Enligt denna uppfinning, vars kannetecken framga av efterfoljande patentansprak och vilken är utarbetad for att Overvinna den ovannananda svarigheten och for att astadkomma ett forbattrat forfarande och en f Orbattrad apparat for sonderdelning av namnda subhalidanga, astadkommes kondenseringseller sonderdelningsoperationen genom att angan bringas i intim kontakt med den smalta aluminiummetallen och kyles, dvs. s att den Mlles vid lamplig temperatur for sonderdelningen eller kondenseringen av ângan, genom att en mangd av small salt Mlles i intim varmeutbyteskontakt med den smilta aluminiummetallen pa ett annat stalle, medan varme avledes fran det smalta saltet. I en speciellt fordelaktig form av uppfinningen Mlles det smalta saltet i en kropp, som flyter pa den smalta aluminiummetallen pa ett stalle, vilket Or i huvudsak isolerat fran subhalidangans bana, medan metallen cirkuleras mellan kondenserings- eller sonderdelningsomradet och ndrheten av saltkroppen. Kylning av det smalta saltet kan astadkommas pa lampligt satt, vid vilket det undvikes att kylror eller andra varmeutvaxlingselement utsattas for beroring med aluminiummetallen. Exempelvis kunna kylslingor eller liknande vara nedsankta i det smalta saltet eller ocksh kan saltet cirkuleras genom yttre kylanordningar. According to this invention, the characteristics of which are set forth in the appended claims and which are designed to overcome the above-mentioned liability and to provide an improved process and an improved apparatus for probing said subhalidanges, the condensing or probing operation is accomplished by bringing the contact into intimate contact with it. melt the aluminum metal and cool, ie. So that it is melted at a suitable temperature for the probe division or condensation of the steam, by mixing a quantity of small salt in intimate heat exchange contact with the molten aluminum metal in another place, while heat is dissipated from the molten salt. In a particularly advantageous form of the invention, the molten salt is ground in a body floating on the molten aluminum metal in a stable, which is substantially isolated from the path of the subhalide, while the metal is circulated between the condensing or probing region and the proximity of the salt body. Cooling of the molten salt can be effected in a suitable manner, in which case cooling pipes or other heat exchange elements are not exposed to contact with the aluminum metal. For example, cooling coils or the like may be immersed in the narrow salt or the salt may also be circulated through external cooling devices.
Ett alternativt tillvagagangssatt bestar i att anvanda ett smdlt salt, vilket ãr tyngre an aluminium. I sa fall kan det smalta saltet anbringas i en brunn eller 1 ett pa annat satt avskilt omrade vid bottnen av en del av den smalta aluminiummassan med lampliga atgarder for avlagsnande av varme fran saltet. An alternative approach consists of using a molten salt, which is heavier than aluminum. In that case, the molten salt may be placed in a well or in another set-aside area at the bottom of a portion of the molten aluminum mass with suitable means for removing heat from the salt.
Den smalta aluminiummetallen cirkuleras, sasom anforts ovan, mellan stallet for subhalidsonderdelning och stallet for kylning genom det smalta saltet flir effektivt avlagsnande av varmet, vilket absorberas genom sonder delnings- eller dissociationsreaktionen. Allteftersom operationen fort& kan smalt aluminium kontinuerligt eller intermittent avledas frail denna metallmassa for att bilda den onskade produkten fran siinderdelningsapparaten. The molten aluminum metal is circulated, as stated above, between the subhalide decomposition site and the refrigeration salt cooling site to effectively dissipate the heat, which is absorbed by the probe decomposition or dissociation reaction. As the operation proceeds, narrow aluminum can be continuously or intermittently diverted from this mass of metal to form the desired product from the sintering apparatus.
Pa den bifogade ritningen visas som exempel vissa utforingsformer av en apparat enligt denna uppfinning, i vilken forfarandet enligt uppfinningen kan genomfOras. Pa ritningen Or fig. 1 en vertikal langdsektion av en utforingsform av en sadan apparat, visad i stor forenkling och schematiskt. Fig. 2 at en partiell horisontalsektion otter linjen 2-2 i fig. 1. Fig. 3 Or en partiell horisontalsektion, liknande fig. 2, och visar ett modifierat kylarrangemang. Fig. 4 Br en partiell vertikalsektion, liknande fig. 1, och visar en annan utforingsform av uppfinningen. The accompanying drawing shows by way of example certain embodiments of an apparatus according to this invention, in which the method according to the invention can be carried out. In the drawing, Fig. 1 is a vertical longitudinal section of an embodiment of such an apparatus, shown in great simplification and schematically. Fig. 2 is a partial horizontal section taken along line 2-2 of Fig. 1. Fig. 3 is a partial horizontal section, similar to Fig. 2, showing a modified cooling arrangement. Fig. 4 shows a partial vertical section, similar to Fig. 1, showing another embodiment of the invention.
Den pa fig. 1 och 2 visade apparaten omf attar ett slutet karl 10, bestaende av eller inklatt med lampligt eldfast material, dvs. material som ar mekaniskt lampligt for andamalet och I huvudsak inert gentemot forstoring genom small aluminium och aluminiumhalider vid de forekommande temperaturerna, och exempel pa sadana material dr kol, grafit, eldfasta material av aluminiumoxidtyp och liknande. Karlet Or konstruerat for upptagande av en avsevard massa av my&et rent smalt aluminium 11, exempelvis till den visade nivan, Over hela sin bottendel, sO. att ytan av den smalta aluminiummetallen dr blottad i sonderdelningsavdelningen eller -kammaren, som allmant betecknas med 12. Sonderdelningskammaren 12 at lampligen fOrsedd med en neat framskjutande skiljevagg eller liknande, sasom den visade skiljevaggen 13, vilken uppdelar kaminaren i en inloppsavdelning 14 och en utlopps- eller stankavdelning 15. Aluminiumsubhalidgas, som infOres genom en inloppsledning 16 Overst i avdelningen 14, strommar salunda in i den senare, under skiljevaggen 13, vilken bestar av samma material som vaggarna 10, och darifran genoin avdelningen 15 till en upptill anbragt utloppsledning 17. The apparatus shown in Figs. 1 and 2 comprises a closed vessel 10, consisting of or enclosed with a suitable refractory material, i.e. materials which are mechanically suitable for the spirit and mainly inert to magnification by small aluminum and aluminum halides at the prevailing temperatures, and examples of such materials are carbon, graphite, alumina type refractories and the like. Karlet Or designed for receiving a considerable mass of pure & narrow pure aluminum 11, for example to the level shown, Over its entire bottom part, sO. that the surface of the narrow aluminum metal is exposed in the probe compartment or chamber, generally designated 12. The probe chamber 12 is suitably provided with a neatly projecting partition or the like, such as the shown partition 13, which divides the chamber into an inlet compartment 14 and an outlet. or stench compartment 15. Aluminum subhalide gas, which is introduced through an inlet duct 16 at the top of the compartment 14, thus flows into the latter, under the separating cradle 13, which consists of the same material as the cradles 10, and thence through the compartment 15 to an upper outlet duct 17.
En roterande omrarare eller propeller 18, anbragt pa en drivaxel 19 och partiellt neddoppande i den smaIta aluminiummetallen, uppratthaller en i huvudsak kontinuerlig dusch eller strale av metallen i kammaravdel- ningen 15. Subhalidgasen strommar salunda igen:om ett omrade, dar strOmmarna och dropparna av metallen Over hela omradet, och rin- nande nedfor vaggarna, astadkomma en stor specifik yta med en temperatur vasentligt under gasens temperatur. Det uppnas darfor ef- fektiv varmeoverforing fran gasen till den smalta metallen f Or astadkommande av den 3 onskade sonderdelnings- eller dissociationsreaktionen, varigenom aluminiumsubhaliden Ater omvandlas till normal aluminiumhalid oeh metalliskt aluminium. Den ater omvandlade aluminiummetallen avlamnas i den stankande metallen och ansamlas salunda i huvudmassan av aluminium 11. A rotary agitator or propeller 18, mounted on a drive shaft 19 and partially immersed in the narrow aluminum metal, maintains a substantially continuous shower or jet of the metal in the chamber compartment 15. The subhalide gas flows like this again: in an area where the currents and droplets of the metal Over the whole area, and running down the rocks, create a large specific surface with a temperature substantially below the temperature of the gas. Therefore, efficient heat transfer from the gas to the molten metal is achieved to produce the desired probing or dissociation reaction, whereby the aluminum subhalide Ater is converted to normal aluminum halide or metallic aluminum. The reconstituted aluminum metal is deposited in the stinking metal and thus accumulates in the main mass of aluminum 11.
Om en skiljeva.gg 13 anvandes, avskiljer den inloppsavdelningen 14 frau den kraftiga stankningen i kanunaravdelningen 15, sa att metallen halles skild Iran inloppsrOret 16 och varje annan kanal, som inmynnar i avdelningen 14. If a separator 13 is used, it separates the inlet compartment 14 from the heavy stench in the cannon compartment 15, so that the metal is kept separate from the inlet pipe 16 and any other channel which opens into the compartment 14.
En kylkammare 20 är anordnad pa ett sane i karlet, exempelvis vid den langst fran utloppsledningen 17 belagna anden, genom en annan skiljevagg 21, som âr dimensionerad sa att den framskjuter vasentligt under ytan av den smalta aluminiummetallen 11, sa att det bildas ett omrade som är isolerat fran den under behandling befintliga huvudgasstrommen och fran turbulensen och stankningen i sOnderdelningskammaren 12. Denna skiljevagg, vilken bestar av 15.mpligt eldfast material liksom de andra delarna av karlet, kan ha en eller flera sma kanaler 22 i narheten av sin Ovre del for utjamning av trycket i kamrarna 12 och 20. A cooling chamber 20 is arranged on a surface in the vessel, for example at the duct furthest from the outlet line 17, through another partition 21, which is dimensioned so that it protrudes substantially below the surface of the narrow aluminum metal 11, so that an area is formed which is insulated from the main gas stream under treatment and from the turbulence and stench in the decomposition chamber 12. This partition, which consists of 15-member refractory material like the other parts of the vessel, may have one or more small channels 22 near its upper part for equalization of the pressure in chambers 12 and 20.
En massa eller ett skikt av small salt 24 flytande pa ytan av den smalta aluminiummetallen i kamamren 20 for avledning av varme fran aluminiummetallen. En varmeutvaxlingsanordning finnes for kylning av det smalta saltet. Exempelvis aro pa fig. 1 kylror 25 anordnade 1 lampliga slingor eller liknande och anordnade sa att de helt och hallet be-. finna sig mom den smalta saltmassan. Genom inlopps- och utloppsforbindningar 26, 27 cirkuleras kylfluidum, sasom vatten, kontinuerligt genom rOren 25 fran en joke visad utvandig kalla. A mass or layer of small salt 24 floating on the surface of the narrow aluminum metal in the chamber 20 to dissipate heat from the aluminum metal. A heat exchange device is provided for cooling the molten salt. For example, in Fig. 1, radiators 25 are arranged in lampable loops or the like and are arranged so that they are completely covered. find yourself mom the narrow mass of salt. Through inlet and outlet connections 26, 27, cooling fluid, such as water, is continuously circulated through the pipe 25 from a joke shown external cold.
Fastan en separat anordning eventuellt kan forekomma tjanar den roterande stankpropellern 18 till att beframj a cirkulation av den smalta aluminiummetallen mellan omradet under sOnderdelningskammaren 12 och kylkammaren 20 for att medverka till att aluminiummetallen Mlles vid den 8nskade temperaturen, som är tillrackligt lag for effektiv varmeabsorption for sonderdelningsoperationen i kammaravdelningen 15. I den som exempel visade apparaten inskjuter propelleraxeln 19 i avdelningen 15 genom ett lampligt tatt lager 30 i en lutande takdel 31 av karlet. AxeIn 19 kringvrides av en lamplig ej visad drivanordning. Propellern och axeln 19 aro konstruerade av eller Overdragna med material, som Mr lamplig styrka och lampligt mot-stand mot smalt aluminium, sasom grafit, bornitrid, kiselkarbid eller kiselnitrid. Propellern 18 är av bladformig eller liknande konstruktion for astadkommande av den onskade duschen eller kaskaden av metall i avdelningen 15 och for astadkommande av kontinuerlig sluten cirkulation i den smalta aluminiummdssan. 11 mellan avdelningen 15 och utrymmet under det smalta saltskiktet 24 i kammaren 20 for att hMla metallen ldmpligt kyld. Although a separate device may be present, the rotary stench propeller 18 serves to promote circulation of the molten aluminum metal between the area below the decomposition chamber 12 and the cooling chamber 20 to assist in the aluminum metal being melted at the desired temperature, which is sufficiently law for efficient heat absorption in the chamber compartment 15. In the apparatus shown as an example, the propeller shaft 19 in the compartment 15 is inserted through a light-bearing bearing 30 into an inclined roof part 31 of the barrel. AxeIn 19 is rotated by a suitable drive device (not shown). The propeller and shaft 19 are constructed of or coated with materials such as light strength and light resistance of narrow aluminum, such as graphite, boron nitride, silicon carbide or silicon nitride. The propeller 18 is of blade-like or similar construction to provide the desired shower or cascade of metal in the compartment 15 and to provide continuous closed circulation in the narrow aluminum mass. 11 between the compartment 15 and the space under the narrow salt layer 24 in the chamber 20 to keep the metal adequately cooled.
Ett utloppsrOr 35 eller annan lamplig anordning kan anva.ndas for att kontinuerligt eller periodiskt avlagsna smalt aluminium fran karlet, sa att i huvudsak samma niva uppratthalles i det senare. Den genom senderdelningsverkan erhdllna produkten avgar salunda i sjalva verket genom rOret 35. An outlet pipe 35 or other suitable device can be used to continuously or periodically remove narrow aluminum from the vessel, so that substantially the same level is maintained in the latter. The product obtained by the transmitter-sharing effect thus actually leaves through the tube 35.
Under inverkan av en ej visad pump medstroms i forhallande till utloppet 17 ledes gasen innehallande aluminiumsubhaliden kontinuerligt till kammaravdelningen 15, dar den kyles av den stankande metallen och under& sonderdelningsreaktionen med atfoljande avlamnande av metalliskt aluminium till badet 11. Den forbrukade gasen avgar genom utloppet 17 och bestar i huvudsak endast av den normala haliden, om processen arbetar med onskad effektivitet for i huvudsak fullstandig sonderdelning av subhaliden. Det i sonderdelningsreaktionen avlagsnade varmet absorberas av den smalta aluminiummetallen 11 och avledes fran den senare av det smalta saltskiktet 24, som i sjalva verket overfor det till det cirkulerande kylmedlet i roren 25. Under the influence of a pump (not shown) co-current relative to the outlet 17, the gas containing the aluminum subhalide is passed continuously to the chamber compartment 15, where it is cooled by the stinking metal and during the subdivision reaction with subsequent deposition of metallic aluminum to the bath 11. consists essentially only of the normal halide, if the process works with the desired efficiency for essentially complete probe division of the subhalide. The heat deposited in the probe division reaction is absorbed by the narrow aluminum metal 11 and is diverted from the latter by the narrow salt layer 24, which in fact opposes it to the circulating refrigerant in the tubes 25.
Exempelvis kan den i ledningen 26 tillforda gasen harrOra fran en lamplig konverter av ovan beskrivet slag och kan innehalla aluminiummonoklorid. Den kan naturligtvis dven innehalla oreagerad normal klorid, dvs, gasformig aluminiumtriklorid. Den ursprungliga omvandlingsreaktionen kan genomforas vid olika temperaturer och tryek, vanligen atmosfarstryck eller under atmosfarstryck. Exempelvis är ett for narvarande foredraget arbetssatt sadant, att temperaturen hos den monokloridhaltiga gasen, som tillfores kammaren 12 har en temperatur av 1000-1200° C eller hogre. Genom sonderdelningsreaktionen vid avledning av varme i avdelningen 15 omvandlas aluminiummonokloriden (A1C1) pa nytt till aluminiumtriklorid och elementart aluminium. Den genom utloppet 17 utmatade gasen bestar salunda foretradesvis av aluminiumtriklorid enbart, vilken kan tillvaratagas eller pa annat salt behandlas fOr fOrnyad anvandning i om-vandlingsreaktionen. For example, the gas in the line 26 may supply the resin from a lamp converter of the type described above and may contain aluminum monochloride. It may, of course, also contain unreacted normal chloride, i.e., gaseous aluminum trichloride. The initial conversion reaction can be carried out at different temperatures and pressures, usually atmospheric pressure or below atmospheric pressure. For example, a presently preferred mode of operation is such that the temperature of the monochloride-containing gas supplied to the chamber 12 has a temperature of 1000-1200 ° C or higher. Due to the heat dissipation reaction in heat dissipation in compartment 15, the aluminum monochloride (A1C1) is converted again to aluminum trichloride and elemental aluminum. The gas discharged through the outlet 17 thus preferably consists of aluminum trichloride alone, which can be recovered or treated with another salt for reuse in the conversion reaction.
Temperaturen hos aluminiummassan 11 och saltskiktet 24 Mlles vid varden, som lampa sig f Or de avsedda kylfunktionerna. Om exempelvis temperaturen hos den i sonderdelningsapparaten inkommande gasen ar 1000-1200° C, kan den smalta aluminiummetallen lamp- 4 ligen lianas vid en temperatur av 700800° C, och for detta andarnal halles den smalta saltlosningen 24 foretradesvis vid en temperatur ay 200-400° C, exempelvis genom cirkulation av kylvatten genom roren 25 vid rumstemperatur. The temperature of the aluminum mass 11 and the salt layer 24 Mlles at the cairn, which illuminates for the intended cooling functions. For example, if the temperature of the gas entering the probe dividing apparatus is 1000-1200 ° C, the molten aluminum metal can be leached at a temperature of 700800 ° C, and for this purpose the narrow saline solution 24 is preferably kept at a temperature of 200-400 ° C. ° C, for example by circulating cooling water through the tubes 25 at room temperature.
Olika salter eller saltblandningar, lampligen inerta och med la.mplig smaltpunkt, kunna anvandas for kylning av skiktet 24, och ett lampligt exempel är en blandning av natriumklorid och ,aluminiumtriklorid, foretradesvis i sadana mangder, att materialet Mlles i fullstandigt smalt form vid en relativt lag temperatur och att forluster genom forangning undvikas. En foredragen mangd av dessa komponenter aro de s. k. jamviktskompositionerna, exempelvis innefattande foljande viktmangder ay NaC1 och A1C13 for de angivna temperaturerna och trycken: Salttemperatur (°C) Tryck (atmosfarer) Saltsammansattning % AlCla% NaC1 330° 1 77 23 250° 1 81 19 200° 1 84 16 220° 0,4 80 Exempel pa andra salter eller saltblandningar, vilka ha tillrackligt lag specifik vikt f8r att flyta p5. aluminiumsmaltan, aro: kaliumkolrid (KCI) och aluminiumtriklorid (A1C13), kalciumklorid (CaC1,) och aluminiumtriklorid samt litiumklorid (LiC1) och aluminiumtriklorid. Various salts or salt mixtures, suitably inert and with a suitable melting point, can be used for cooling the layer 24, and a suitable example is a mixture of sodium chloride and, aluminum trichloride, preferably in such amounts that the material Mlles in a completely narrow form at a relatively low temperature and that losses due to evaporation are avoided. A preferred amount of these components are the so-called equilibrium compositions, for example comprising the following amounts of weight ay NaCl and AlCl 3 for the indicated temperatures and pressures: Salt temperature (° C) Pressure (atmospheres) Salt composition% AlCl 3% NaCl 330 ° 1 77 23 250 ° 1 81 19 200 ° 1 84 16 220 ° 0.4 80 Examples of other salts or salt mixtures, which have a sufficiently specific weight to flow p5. aluminum malt, aro: potassium chloride (KCl) and aluminum trichloride (AlCl3), calcium chloride (CaCl2) and aluminum trichloride and lithium chloride (LiCl) and aluminum trichloride.
Fig. 3 visar ett annat sat ati kyla del saltet 24 i kammaren 20, namligen genom utvandig cirkulering av saltblandningen i flytande form genom ett ror 40, en kylanordning 41, exempelvis av radiatortyp, och darefter genom. ror 42 och 43 tillbaka till kammaren 24, dvs. vid motsatt sida. Donna cirkulation astadkommes genom en lamplig anordning, sasom en pump 45 i rorledningarna 42, 43. Fig. 3 shows another sat ati part of the salt 24 in the chamber 20, namely by external circulation of the salt mixture in liquid form through a tube 40, a cooling device 41, for example of radiator type, and then through. tubes 42 and 43 back to the chamber 24, i.e. on the opposite side. Donna circulation is provided by a suitable device, such as a pump 45 in the pipelines 42, 43.
I vissa fall kan ett smalt salt eller saltblandning anvandas, som har hogre tathet an aluminiumsmaltan. Salunda visas pa fig. 4 ett arrangemang innefattande ej endast en skiljevagg 21a, som skiljer kammaren 20 frail sonderdelningskammaren, utan aven en anordning for uppratthallande av ett under aluminiumsmaltan befintligt skikt 47 av smalt salt, som dr avskilt fran turbulensen frail propellern 18. Derma anordning kan vara en behallare eller brunn under den normala golvnivan i karlet 11. Fig. 4 visar en skiljevagg 48 av eldfast material mittfor den ovre skilj evaggen 21a och strackande sig uppat Iran karlets golv. Liksom pa fig. 1-3 aro lampliga kylanordningar for den smalta saltmassan anord nade, exempelvis kylror 49 motsvarande roren 25. In some cases a narrow salt or salt mixture can be used which has a higher density than the aluminum malt. Thus, Fig. 4 shows an arrangement comprising not only a partition wall 21a, which separates the chamber 20 from the probe dividing chamber, but also a device for maintaining a layer 47 of narrow salt present under the aluminum malt, which is separated from the turbulence from the propeller 18. This device may be a container or well below the normal floor level in the tub 11. Fig. 4 shows a separating cradle 48 of refractory material opposite the upper separating cradle 21a and extending upwards to the floor of the tub. As in Figs. 1-3, suitable cooling devices for the narrow salt mass are provided, for example cooling pipes 49 corresponding to the pipes 25.
Den i samband med fig. 4 anvanda proceduren kr i huvudsak densamma som beskrivits. Sonderdelningen astadkommes i stankkammaravdelningen 15 och den smalta aluminiummetallen cirkuleras medelst propellern (liksom i fig. 1) till varmeutvaxlingsforhallande med det smalta saltet 47 for bortledning av varmet frail sanderdelningsreaktionen. Ett exempel pa en lamplig saltblandning, lampligen inert gentemot flytande aluminium, och med hogre specifik vikt an det senare, är bariumbromid och aluminiumtribromid, exempelvis i viktproportionerna 28 % BaBr, och 72 % AlBr3. The procedure used in connection with Fig. 4 is essentially the same as described. The probe division is effected in the stench chamber compartment 15 and the narrow aluminum metal is circulated by means of the propeller (as in Fig. 1) to heat exchange ratio with the narrow salt 47 to dissipate the heat from the sand division division reaction. An example of a suitable salt mixture, suitably inert to liquid aluminum, and with a higher specific gravity than the latter, is barium bromide and aluminum tribromide, for example in the weight proportions of 28% BaBr, and 72% AlBr3.
Medan i vissa fall, speciellt yid arrangemangen enligt fig. 1-3, karldelen, som innehailer det smalta saltet, kan vara oppen till atmosfaren och skiljevaggen 21 operforerad, är arrangemanget med den slutna kammaren 20 med tryckutjamningsoppningen 22 fordelaktigt och det Sr faktiskt nOdvandigt, nar den subhalidhaltiga gasen alstras och tillf8res vid ett tryck avsevart under atmosfarstrycket. While in some cases, especially in the arrangements of Figs. 1-3, the male portion containing the narrow salt may be open to the atmosphere and the septum 21 unperforated, the arrangement of the closed chamber 20 with the pressure equalization orifice 22 is advantageous and it is actually necessary. when the subhalide-containing gas is generated and supplied at a pressure substantially below atmospheric pressure.
De beskrivna procedurerna och apparaterna erbjuda ett effektivt salt att utvinna aluminium genom sonderdelning av subhaliden, sasom aluminiummon:oklorid eller aluminiummonobromid i gasform under effektivt avlagsnande av sonderdelningsvarmet och under undvikande av att aluminiummetallen utsattes for kylmedel, som skulle kunna fororena den. The described procedures and apparatus offer an efficient salt to extract aluminum by probing the subhalide, such as aluminum monochloride or gaseous aluminum monobromide while effectively dissipating the probing heat and avoiding exposure to the aluminum metal which could contaminate it.
Uppfinningen skall icke vara begransad till de hdr speciellt beskrivna utforingsformerna, utan den kan genomforas pa andra satt mom ramen for de efterfoljande patentanspraken. The invention is not to be limited to the embodiments specifically described herein, but may be practiced in other ways within the scope of the appended patent claims.
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