US3900312A - Reduction of aluminum chloride by manganese - Google Patents
Reduction of aluminum chloride by manganese Download PDFInfo
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- US3900312A US3900312A US297695A US29769572A US3900312A US 3900312 A US3900312 A US 3900312A US 297695 A US297695 A US 297695A US 29769572 A US29769572 A US 29769572A US 3900312 A US3900312 A US 3900312A
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- United States
- Prior art keywords
- manganese
- aluminum
- chloride
- elemental
- liquid
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 66
- 239000011572 manganese Substances 0.000 title claims abstract description 65
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 48
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 14
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 14
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 14
- 239000011565 manganese chloride Substances 0.000 claims abstract description 14
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 12
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 claims description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims 1
- 229910001626 barium chloride Inorganic materials 0.000 claims 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims 1
- 239000001110 calcium chloride Substances 0.000 claims 1
- 229910001628 calcium chloride Inorganic materials 0.000 claims 1
- 235000011148 calcium chloride Nutrition 0.000 claims 1
- 229910001629 magnesium chloride Inorganic materials 0.000 claims 1
- 239000001103 potassium chloride Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 description 26
- 239000002184 metal Substances 0.000 description 26
- 239000007787 solid Substances 0.000 description 23
- 239000010936 titanium Substances 0.000 description 16
- 102100026194 C-type lectin domain family 2 member B Human genes 0.000 description 15
- 101000912618 Homo sapiens C-type lectin domain family 2 member B Proteins 0.000 description 15
- 229910001510 metal chloride Inorganic materials 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 10
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 229910052719 titanium Inorganic materials 0.000 description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 9
- 239000003638 chemical reducing agent Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 230000002349 favourable effect Effects 0.000 description 6
- 150000002739 metals Chemical class 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- -1 NaCl Chemical class 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000001805 chlorine compounds Chemical class 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229910018575 Al—Ti Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- 229910006639 Si—Mn Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000010006 flight Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1277—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using other metals, e.g. Al, Si, Mn
-
- 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
- C22B21/0053—Obtaining aluminium by other processes from other aluminium compounds
- C22B21/0061—Obtaining aluminium by other processes from other aluminium compounds using metals, e.g. Hg or Mn
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1268—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams
- C22B34/1272—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/06—Dry methods smelting of sulfides or formation of mattes by carbides or the like
Definitions
- the manganese reduces the liquid aluminum chloride and forms essen- [56] References Cited tially elemental aluminum and manganese chloride.
- the temperature range is between 180600C and the pressure range is 15-450 psia.
- the primary object of the present invention is to produce a metal by direct reduction of a chloride of that metal by a reductant metal which is in the solid state during the reaction.
- a still further important object of the present invention is to produce silicon by reducing SiCl in either liquid or gaseous state by manganese or aluminum in solid state.
- FIG. I shows in diagrammatic form an apparatus for carrying out the invention when the metal chloride is gaseous
- FIG. 2 shows in diagrammatic form an apparatus for carrying out the invention in a batch process when the metal chloride is liquid
- FIG. 3 shows in diagrammatic form a further appara tus for carrying out the invention in a batch process when the metal chloride is liquid;
- FIG. 4 shows in diagrammatic form an apparatus for carrying out the invention in a continuous process when the metal chloride is liquid.
- the instant invention has extremely broad applicability.
- the scope of the invention deals with reacting a fluid metal chloride with a solid reductant powder.
- the most important criteria is that the reductant metal powder is in solid form and the metal chloride be in fluid form at the temperature and pressure that the process is carried out at.
- Table I shows the various melting points (M.P.) and boiling points (B.P.),of various metals and their chlorides as well as their free energies at 298K', 500K and 700K. From this Table, one skilled in the artcan dey duct the operating parameters for carrying out the instant inventive process.
- any I i TABLE I Properties of Metals and Metal Chlorides I Metal AF,, Kcal/gmolc Metal M.P..K B.P..K Chloride M.P..K B.P..l ⁇ ' 298K 5()(lK 7()()K Aluminum(Al) 931.7 260( AICL, 465.6 720 -l53.() l44.5 1 38.6 Beryllium (Be) 1556 3243 BeCl 678 (S20)- ('l()2.9) 96.6) Calcium (Ca) 1124 1760 CaCl.
- FIG. 1 diagrammatically shows a low temperature gaseous AlCL, apparatus, a reactor 26 and AlCL, generator 22 are integrated in one horizontal inch alumina tube 19. Each section'ofthe tube 19 is separated by pyrex wool 28 and an 8-inch void space 24.
- the AlCl generator section 22 contains a l inch long bed of aluminum pellets.
- the reactor sec: tion 26 contains a /2-inch long bed of 5 grams of manganese.
- the condenser 32 is a 2-inch diameter mild steel pipe 5 inches long which is connected to the ceramic tube with a packing 'gland30 and has a conduit 34 and valve 36 for vcnting' any gases.'The reactor and generator sections of the tube are heated separately with resistance wire 20.
- Chlorine vapor from source l0 is passed d vija conduit 12 through a rotometer 14 to measure the flow rate which is controlled by valve 16 and is passed through conduit 18 into the aluminum pellets in generator 22 to generate AlCl at 300C.
- the AICL then passes through the bed of Mn in reactor 26 which ranges in particlesize from 45 to 300 microns (all on 325 mesh).
- the particle size of the Mn was chosen for a size distribution of high surface area'to ensure good gas-solid contact. Runs were typically made for 2 hours with 5 grams of Mn at 300 to 600C and an AlCl flow rate or 3 grams/hour with the following results:
- the process could be carried out in conventional gassolid reactors and combinations thereof.
- the MnCl could be removed from the aluminum product by vaporization as an MnCI -AICL, gas complex or by dissolving in liquid AICL, or another solvent.
- the reaction could be stopped at any degree of Al production and the aluminum then produced separated from the Mn by means such as aluminum subhalide distillation, zinc extraction, zone freezing, or differential vaporization.
- EXAMPLE 11' A simplified diagram of a low-temperature liquid AICL, laboratory apparatus is shown in FIG. 2.
- a batch reactor 40 is designed to effectively contact Mn metal granules with liquid AICL, in a continuously agitated vessel.
- the apparatus is designed to operate for various lengths of time at l80600C and 14.7-450 psia, with approximately 30-60 grams Mn and 120-450 grams AlCl charge.
- the reactor 40 contains a 2 [2-inch diameter alumina tube 58 which is housed in a 3-inch diameter stainless steel pipe 60 and heated externally by resistance wires 62.
- a stainless-steel stirrer 56 and shaft 54 along with a motor 50 is mounted in place on the top flange 46 with a packing gland 48.
- the charge is introduced thro ugh conduit 44.
- a pressure gauge 52 is mounted on conduit 42. Following the reaction period, the unreacted AICL, is boiled off through conduit 64, valve 66, into condenser 68 which is vented by conduit 70 and valve 72.
- the liquid AlCl serves as a solvent to dissolve the solid MnCl that is formed at the reaction interface along with the aluminum, thus resulting in a A porous aluminum microstructure, through which liquid AlCl gains ready access to the unreacted manganese within.
- porosity namely, the volume of the MnCl and aluminum products would greatly exceed that of the substrate dense manganese so that a tendency would exist for the film of solid reaction products or of the porous aluminum to expand away from the manganese and to thereby add to the porosity.
- reaction lies in the increase in boiling point of the AlCl MnCl liquor as the reaction proceeds due to increased concentration of MnCl- This permits use of beneficial higher temperatures for the reaction up to 600C instead of being limited by about 352.5C, the critical temperature of pure AlCl This increased temperature factor thus can be used to readily compensate for any decreasing AlCl concentration due to increase of MnClcontent as the reaction progresses. Additional MnCl or other soluble metal salts, could be added as needed to establish optimum conditions.
- An advantage of the liquid AICL, process lies in the ease of separation of the products formed.
- the density decreases from about 7.4g/ml for Mn to 2.7g/ml for A1.
- the finished product can be readily separated by utilization of the vast difference in density.
- the product could be carried out of a continuous reactor in the liquor stream at appropriate velocity leaving Mn-containing particles behind; or conventional gravity separation devices could be employed, with recycling of the Mn-contaiining particles.
- all the manganese could be replaced with aluminum in the reactor or series of reactors to obviate the need for separation :of the aluminum from an intermediate.
- the product aluminum can be cleansed of adherent MnCl by a wash of fresh liquid AlCl in which the MnCl is soluble in AlCl to 50% by weight MnCl the two salts can be readily separated by crystallization, sublimation or by evaporation of the AICI Water or organic solvents can also be used to remove any resid ual MnCl or AlCl
- the AlCl which is left on the surface of the aluminum can be removed readily by sublimation or evaporation.
- the MnCl can be removed from AICL, liquor by evaporating the latter with its 180C atmospheric boiling point versus 1190C for the boiling point of MnCl. or the MnCl can be crystallized out of a hot concentrated solution of MnCl and AlCl by reducing the temperature.
- the AICIa, after removal of the MnCl can be reused.
- An unexpected advantage of the reaction with liquid AICI is the formation of the aluminum over the surface of the manganese metal in a manner that does not block reaction. This affords the opportunity of cutting short the reaction at any desired time and still being temperature of the aluminum metal canbe brought slightly over its melting point to cause the aluminum to flow from the particles and be collected. leaving the residue of manganese metal with a slight film of high melting point manganesealuminum alloy at theinterface. The manganese. residue is returned to the reactor or if the particle size is very small, it can be agglomerated first.
- Agitation of an abrasive or impact nature can cause the aluminum coating to separate for collection. Furthermore, more unreacted manganese will be exposed.
- the aluminum can be separated from the manganese by conventional methods such as subhalide or zine extraction.
- This particular aspect of the invention may be practiced in many forms. Firstly, it is amenable to many conventional solid-liquid contactors, reactors and flow arrangements such as fluid, static and moving bed reactors, batch reactors, and cyclone and tube transport reactors, all in concurrent, countercurrent, semicontinuous or batch arrangements. Agitation may be performed by stirrers, flow or recirculation of slurry, vibrators, shakers, or the recycling of an inert gas or liquid AlCl rotating or tumbling drums with or without flights, grinding balls, or other obvious means.
- FIG. 3 is a schematic diagram illustrating an apparatus for performing the process of the present invention in a batch-wise manner.
- the process uses a noncorrosive metal or ceramic lined steel reactor 80 having heating means such as electric heating coils 82 for control of the temperature necessary to maintain the AlCl in a liquid state and provide other heat demands.
- the reactor is charged with AICL, and manganese from the top through charge and discharge port 84. Generally, an excess of AlCl will be present to keep the reactants in the form of a solid-liquid slurry.
- the reactor is sealed and heated to reaction temperature.
- the AICL At temperature (l80-600C), the AICL, is liquid and exhibits a vapor pressure of l-45O psia depending on the exact reactor temperature and composition of the liquor.
- the mixture of reactants is maintained at temperature and pressure until all of the manganese has been consumed to form aluminum metal and MnCl
- the mixture is meehanically. stirred by a blade 88 attached to a shaft 86, powered by a motor (not shown) to enhance contact and reduce reaction time.
- any excess AlCl is removed by opening the reactor and bleeding off the AlCl;, as a gas through conduit 90 and valve 92. Removal can be enhanced by pulling a vacuum on the reactor and/or by increasing the temperature.
- the aluminum and MnClare discharged as solids and subsequently separated by means such as melting, vaporization, or solvent extraction.
- EXAMPLE IV An apparatus for performing the process of the present invention in a continuous manner is illustrated in FIG. 4.
- the process uses a corrosion-resistant or ceramic-lined steel counter-current reaction tower 100 having heating means 102 for maintaining the AlCl;,- MnCl solution in the liquid state at from l80-600C 8 and 15-450 psia.
- Granular solid manganese is continuously introduced from the top at input port 104 and AICL, is continuously introduced from the bottom at input port 106 in the countercurrent reactor.
- the solid aluminum product is continuously removed from the bottom at I10 andthc MnCl from the top at 108 and- /or bottom at 1 10, depending on the extent to which it dissolves in the AICI TiCL, AND MAGNESIUM Liquid TiCL, can be reduced by solid powdered magnesium.
- powdered magnesium and TiCl 4 can be simultaneously charged into a reactor as above discussed, heated to 200-650C at a pressure from 0-676 psia and reacted to give titanium metal comixed, adhering to, or alloyed with unreacted magnesium, if any, and MgCl Under these conditions, magnesium is solid, titanium is solid, MgCl in pure form is solid, and TiCl is liquid if the total pressure is above the vapor pressure of TiCl (critical temperatures 365C).
- thermodynamics of this reaction is favorable. For example, at 500K the thermodynamics show the reduction reaction to be quite favorable:
- TiCl AND MANGANESE Liquid or gaseous TiCl can be reduced by solid powdered manganese in accordance with:
- the tem perature range over which the reaction is favorable is from -30C (the melting point of TiCl to about l600C realizing that above about 1 175C some of the manganese will be in liquid phase due to a Ti-Mn eutectic of that melting point.
- the preferred pressure range is from 0-676 psia.
- the critical point of TiCl is 365C and 46 atmospheres; however, at high termperatures, vapor pressure lowering .d'ue to the presence of otheririert metal salts such as NaCl, CaCl- KCL, MgCL. 350,, etc. allows TiCl, to remain in the liquid state.
- the reaction proceeds favorably with TiCl in the gaseous state. Typical experimental results are shown in EXAMPLE V.
- Liquid or gaseous SiCl can be reduced by solid powdered manganese in accordance with:
- the temperature range over which the reaction is favorable is from C (the melting point of SiCl to about 1600C realizing that above about l040C some of the manganese will be in liquid phase due to a Si-Mn eutectic of that melting point.
- the critical point of SiCl is 234C and 37 atmospheres. Above the critical temperature the SiCl, will bea vapor unless a suitable inert metal salt such as NaCl, CaCl KC], MgCl- BaCl etc, allows SiCl to remain in the liquid state. In addition, the reaction proceeds favorably in the gaseous state.
- SiCl AND ALUMINUM Liquid or gaseous SiCl can also be reduced by solid powdered aluminum in accordance with:
- the temperature range over which the reaction is favorable is from 70C (the melting point of SiCl to about 577C realizing that above about 577C the aluminum will be in the liquid phase due to a Si-Al eutectic of that melting point.
- Above 234C the critical temperature of SiCl SiCl, will be a vapor unless a suitable inert metallic salt such as NaCl, CaCl KCl, MgCl BaCl etc. allows the SiCl to remain in the liquid state.
- EXAMPLE V The following typical experimental results obtained from the apparatus shown in FIG. 2 demonstrate the production of Ti and Si metals from their respective chlorides.
- the reactor was charged with 60 grams of -100, +200 mesh electrolytic manganese and 410 grams of reagent grade TiCl The reactor was heated to 336C for 3 hours while agitating with a paddle shaped stirrer at 300 rpm under a TiCl vapor pressure of 425-443 psig. After 3 hours the TiCl was bled from the reactor into a condenser. The hot reactor was then purged with argon and cooled to room temperature. The solid residue in the reactor was removed and analyzed for titanium metal. A total of 3.18 grams of titanium metal was found.
- the reactor was charged with 60 grams of -l00, +200 mesh aluminum powder and 695 grams of reagent grade SiCl The reactor was heated to 200C for 3 hours while agitating at 1200 rpm with a turbine shaped stirrer under a SiCl vapor pressure of 388 psia. After 3 hours the SiCl was bled from the reactor into a condenser. The reactor was cooled to room temperature at which time the solid residue was removed and analyzed for silicon metal. A total of 2.13 grams of silicon metal was found.
- the free energies of reaction using manganese as the reductant are A 50" 29.25Kcal and A G 30. IOKcal per mole of Ti formed as calculated from the following stoichiometric reaction:
- AICL can be continuously removed by throttling TiCl into and out of the system carrying AlCL, with 10 it.
- the MnCl zproduced by reaction of TiCl with Mn cannot be removed so easily on a continuous basis.
- inert metallic salts of low volatility, especially metal halides are beneficial in carrying out the reactions above described.
- the inert metallic salts are used to lower the vapor pressure of the metal chloride, e.g. AICL TiCh, SiCl so that a higher temperature can be reached in the closed reactor at a given pressure.
- a process for producing aluminum in essentially elemental form comprising the steps of providing aluminum chloride, which chloride is in a liquid phase; providing elemental manganese in solid phase; reacting said liquid aluminum chloride and elemental manganese in a vessel at a pressure and at a temperature up to 350C at which they will maintain their respective phases, the elemental manganese reducing the liquid aluminum chloride and forming essentially elemental aluminum and manganese chloride.
- reaction is carried out in a temperature range between l350C and pressure range of from 14-450 psia.
- a process for producing aluminum in essentially elemental form comprising the steps of a. providing aluminum chloride in a liquid phase;
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Priority Applications (21)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US297695A US3900312A (en) | 1972-10-16 | 1972-10-16 | Reduction of aluminum chloride by manganese |
DE19732348450 DE2348450A1 (de) | 1972-10-16 | 1973-09-26 | Verfahren zur gewinnung eines metalls |
IT29602/73A IT995540B (it) | 1972-10-16 | 1973-10-01 | Riduzione di cloruro metallico con metallo in polvere |
ZA737706A ZA737706B (en) | 1972-10-16 | 1973-10-02 | Reduction of metallic chloride by powered metal |
AT849873A ATA849873A (de) | 1972-10-16 | 1973-10-04 | Verfahren zum gewinnen von aluminium |
AU61004/73A AU482513B2 (en) | 1972-10-16 | 1973-10-04 | Reduction of metallic chloride by solid metal |
IS2178A IS948B6 (is) | 1972-10-16 | 1973-10-05 | Breyting á málmkenndu klóri með duftkenndum málmi |
BE136454A BE805797A (fr) | 1972-10-16 | 1973-10-08 | Reduction de chlorures metalliques par un metal en poudre |
NO3948/73A NO134304C (ja) | 1972-10-16 | 1973-10-11 | |
OA55037A OA04493A (fr) | 1972-10-16 | 1973-10-13 | Réduction de chlorures métalliques par un métal en poudre. |
IL43428A IL43428A (en) | 1972-10-16 | 1973-10-15 | Reduction of metallic chloride by powdered metal |
FR7336935A FR2202946B1 (ja) | 1972-10-16 | 1973-10-16 | |
RO7376351A RO67591A (ro) | 1972-10-16 | 1973-10-16 | Procedeu de obtinere a aluminiului |
GB4812073A GB1419450A (en) | 1972-10-16 | 1973-10-16 | Production of aluminium from aluminium chloride |
HUAI229A HU167894B (ja) | 1972-10-16 | 1973-10-16 | |
ES419700A ES419700A1 (es) | 1972-10-16 | 1973-10-16 | Procedimiento para la produccion de un metal. |
NL7314252A NL7314252A (ja) | 1972-10-16 | 1973-10-16 | |
BR8093/73A BR7308093D0 (pt) | 1972-10-16 | 1973-10-16 | Processo de reducao de cloreto metalico por metal em po |
JP48116256A JPS4974109A (ja) | 1972-10-16 | 1973-10-16 | |
AR250546A AR201746A1 (es) | 1972-10-16 | 1973-10-16 | Procedimiento para la produccion de un metal elemental |
DD174088A DD108324A5 (ja) | 1972-10-16 | 1973-10-16 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US297695A US3900312A (en) | 1972-10-16 | 1972-10-16 | Reduction of aluminum chloride by manganese |
Publications (1)
Publication Number | Publication Date |
---|---|
US3900312A true US3900312A (en) | 1975-08-19 |
Family
ID=23147359
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US297695A Expired - Lifetime US3900312A (en) | 1972-10-16 | 1972-10-16 | Reduction of aluminum chloride by manganese |
Country Status (20)
Country | Link |
---|---|
US (1) | US3900312A (ja) |
JP (1) | JPS4974109A (ja) |
AR (1) | AR201746A1 (ja) |
AT (1) | ATA849873A (ja) |
BE (1) | BE805797A (ja) |
BR (1) | BR7308093D0 (ja) |
DD (1) | DD108324A5 (ja) |
DE (1) | DE2348450A1 (ja) |
ES (1) | ES419700A1 (ja) |
FR (1) | FR2202946B1 (ja) |
GB (1) | GB1419450A (ja) |
HU (1) | HU167894B (ja) |
IL (1) | IL43428A (ja) |
IS (1) | IS948B6 (ja) |
IT (1) | IT995540B (ja) |
NL (1) | NL7314252A (ja) |
NO (1) | NO134304C (ja) |
OA (1) | OA04493A (ja) |
RO (1) | RO67591A (ja) |
ZA (1) | ZA737706B (ja) |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4035180A (en) * | 1976-03-16 | 1977-07-12 | Toth Aluminum Corporation | Catalytic process for the reduction of aluminum chloride by manganese |
US4106928A (en) * | 1976-03-15 | 1978-08-15 | Westinghouse Electric Corp. | Chlorination process for producing aluminum |
US6284316B1 (en) * | 1998-02-25 | 2001-09-04 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US6433434B1 (en) | 1998-02-25 | 2002-08-13 | Micron Technology, Inc. | Apparatus having a titanium alloy layer |
US20040123700A1 (en) * | 2002-12-26 | 2004-07-01 | Ling Zhou | Process for the production of elemental material and alloys |
US20060183958A1 (en) * | 2003-04-01 | 2006-08-17 | Breneman William C | Process for the treatment of waste metal chlorides |
US20060191372A1 (en) * | 2003-07-04 | 2006-08-31 | Jawad Haidar | Method and apparatus for the production of metal compounds |
EP1999285A1 (en) * | 2006-03-27 | 2008-12-10 | Commonwealth Scientific and Industrial Research Organisation | Apparatus and methods for the production of metal compounds |
US20110091350A1 (en) * | 2008-04-21 | 2011-04-21 | Jawad Haidar | Method and apparatus for forming titanium-aluminium based alloys |
US8834601B2 (en) | 2009-12-18 | 2014-09-16 | Commonwealth Scientific And Industrial Research Organisation | Method for producing low aluminium titanium-aluminium alloys |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6067603A (ja) * | 1983-09-21 | 1985-04-18 | Toho Aen Kk | 金属超微粉の処理方法 |
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US2452665A (en) * | 1944-03-31 | 1948-11-02 | Electro Metallurgical Co | Process for the separation of metals |
US2847205A (en) * | 1954-10-13 | 1958-08-12 | Nat Res Corp | Production of metals |
US3161500A (en) * | 1961-08-04 | 1964-12-15 | Aluminium Lab Ltd | Protection of graphite surfaces from attack by aluminum monohalide |
US3455678A (en) * | 1967-01-16 | 1969-07-15 | Ethyl Corp | Process for the concurrent production of aif3 and a metallic titanium product |
-
1972
- 1972-10-16 US US297695A patent/US3900312A/en not_active Expired - Lifetime
-
1973
- 1973-09-26 DE DE19732348450 patent/DE2348450A1/de active Pending
- 1973-10-01 IT IT29602/73A patent/IT995540B/it active
- 1973-10-02 ZA ZA737706A patent/ZA737706B/xx unknown
- 1973-10-04 AT AT849873A patent/ATA849873A/de not_active Application Discontinuation
- 1973-10-05 IS IS2178A patent/IS948B6/is unknown
- 1973-10-08 BE BE136454A patent/BE805797A/xx unknown
- 1973-10-11 NO NO3948/73A patent/NO134304C/no unknown
- 1973-10-13 OA OA55037A patent/OA04493A/xx unknown
- 1973-10-15 IL IL43428A patent/IL43428A/en unknown
- 1973-10-16 ES ES419700A patent/ES419700A1/es not_active Expired
- 1973-10-16 JP JP48116256A patent/JPS4974109A/ja active Pending
- 1973-10-16 BR BR8093/73A patent/BR7308093D0/pt unknown
- 1973-10-16 AR AR250546A patent/AR201746A1/es active
- 1973-10-16 GB GB4812073A patent/GB1419450A/en not_active Expired
- 1973-10-16 FR FR7336935A patent/FR2202946B1/fr not_active Expired
- 1973-10-16 NL NL7314252A patent/NL7314252A/xx unknown
- 1973-10-16 RO RO7376351A patent/RO67591A/ro unknown
- 1973-10-16 HU HUAI229A patent/HU167894B/hu not_active IP Right Cessation
- 1973-10-16 DD DD174088A patent/DD108324A5/xx unknown
Patent Citations (4)
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US2452665A (en) * | 1944-03-31 | 1948-11-02 | Electro Metallurgical Co | Process for the separation of metals |
US2847205A (en) * | 1954-10-13 | 1958-08-12 | Nat Res Corp | Production of metals |
US3161500A (en) * | 1961-08-04 | 1964-12-15 | Aluminium Lab Ltd | Protection of graphite surfaces from attack by aluminum monohalide |
US3455678A (en) * | 1967-01-16 | 1969-07-15 | Ethyl Corp | Process for the concurrent production of aif3 and a metallic titanium product |
Cited By (27)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4106928A (en) * | 1976-03-15 | 1978-08-15 | Westinghouse Electric Corp. | Chlorination process for producing aluminum |
US4035180A (en) * | 1976-03-16 | 1977-07-12 | Toth Aluminum Corporation | Catalytic process for the reduction of aluminum chloride by manganese |
US7443032B2 (en) | 1998-02-25 | 2008-10-28 | Micron Technology, Inc. | Memory device with chemical vapor deposition of titanium for titanium silicide contacts |
US6284316B1 (en) * | 1998-02-25 | 2001-09-04 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US6433434B1 (en) | 1998-02-25 | 2002-08-13 | Micron Technology, Inc. | Apparatus having a titanium alloy layer |
US8456007B2 (en) | 1998-02-25 | 2013-06-04 | Round Rock Research, Llc | Chemical vapor deposition of titanium |
US6830820B2 (en) | 1998-02-25 | 2004-12-14 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US6830838B2 (en) | 1998-02-25 | 2004-12-14 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US6903462B2 (en) | 1998-02-25 | 2005-06-07 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US6940172B2 (en) | 1998-02-25 | 2005-09-06 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US20090039517A1 (en) * | 1998-02-25 | 2009-02-12 | Micron Technology, Inc. | Chemical vapor deposition of titanium |
US20050255698A1 (en) * | 1998-02-25 | 2005-11-17 | Micron Technology, Inc. | Chemical vapor deposition of titanim |
AU2003293544B2 (en) * | 2002-12-26 | 2010-03-11 | Millenium Inorganic Chemicals, Inc. | Process for the production of elemental material and alloys |
WO2004060594A1 (en) * | 2002-12-26 | 2004-07-22 | Millenium Inorganic Chemicals, Inc. | Process for the production of elemental material and alloys |
US20040123700A1 (en) * | 2002-12-26 | 2004-07-01 | Ling Zhou | Process for the production of elemental material and alloys |
US6955703B2 (en) * | 2002-12-26 | 2005-10-18 | Millennium Inorganic Chemicals, Inc. | Process for the production of elemental material and alloys |
US20060183958A1 (en) * | 2003-04-01 | 2006-08-17 | Breneman William C | Process for the treatment of waste metal chlorides |
US8562712B2 (en) | 2003-07-04 | 2013-10-22 | Commonwealth Sci. and Ind. Res. Org. | Method and apparatus for the production of metal compounds |
US20060191372A1 (en) * | 2003-07-04 | 2006-08-31 | Jawad Haidar | Method and apparatus for the production of metal compounds |
US20090165597A1 (en) * | 2006-03-27 | 2009-07-02 | Commonwealth Scientific And Industrial Research Or | Apparatus and Methods for the Production of Metal Compounds |
EP1999285A4 (en) * | 2006-03-27 | 2010-05-12 | Commw Scient Ind Res Org | APPARATUS AND METHODS FOR PRODUCING METAL COMPOUNDS |
EP1999285A1 (en) * | 2006-03-27 | 2008-12-10 | Commonwealth Scientific and Industrial Research Organisation | Apparatus and methods for the production of metal compounds |
US8821612B2 (en) | 2006-03-27 | 2014-09-02 | Commonwealth Scientific And Industrial Research Organisation | Apparatus and methods for the production of metal compounds |
US20110091350A1 (en) * | 2008-04-21 | 2011-04-21 | Jawad Haidar | Method and apparatus for forming titanium-aluminium based alloys |
US8632724B2 (en) * | 2008-04-21 | 2014-01-21 | Commonwealth Sci. and Ind. Res. Org. | Method and apparatus for forming titanium-aluminium based alloys |
US9080224B2 (en) | 2008-04-21 | 2015-07-14 | Commonwealth Science And Industrial Research Organization | Method and apparatus for forming titanium-aluminium based alloys |
US8834601B2 (en) | 2009-12-18 | 2014-09-16 | Commonwealth Scientific And Industrial Research Organisation | Method for producing low aluminium titanium-aluminium alloys |
Also Published As
Publication number | Publication date |
---|---|
RO67591A (ro) | 1981-08-17 |
FR2202946A1 (ja) | 1974-05-10 |
DD108324A5 (ja) | 1974-09-12 |
BR7308093D0 (pt) | 1974-07-11 |
NO134304C (ja) | 1976-09-15 |
BE805797A (fr) | 1974-04-08 |
ATA849873A (de) | 1976-11-15 |
AU6100473A (en) | 1975-04-10 |
IL43428A (en) | 1976-05-31 |
NO134304B (ja) | 1976-06-08 |
DE2348450A1 (de) | 1974-04-25 |
IS2178A7 (is) | 1973-11-02 |
ZA737706B (en) | 1974-08-28 |
ES419700A1 (es) | 1976-04-16 |
FR2202946B1 (ja) | 1977-09-09 |
IT995540B (it) | 1975-11-20 |
IS948B6 (is) | 1976-08-09 |
HU167894B (ja) | 1976-01-28 |
IL43428A0 (en) | 1974-01-14 |
GB1419450A (en) | 1975-12-31 |
JPS4974109A (ja) | 1974-07-17 |
NL7314252A (ja) | 1974-04-18 |
AR201746A1 (es) | 1975-04-15 |
OA04493A (fr) | 1980-03-30 |
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