FR2245569A1 - Crystalline aluminium hydride prepn - by slow distillation of an ether/aromatic solvent soln - Google Patents
Crystalline aluminium hydride prepn - by slow distillation of an ether/aromatic solvent solnInfo
- Publication number
- FR2245569A1 FR2245569A1 FR7334979A FR7334979A FR2245569A1 FR 2245569 A1 FR2245569 A1 FR 2245569A1 FR 7334979 A FR7334979 A FR 7334979A FR 7334979 A FR7334979 A FR 7334979A FR 2245569 A1 FR2245569 A1 FR 2245569A1
- Authority
- FR
- France
- Prior art keywords
- ether
- soln
- aromatic solvent
- aluminium hydride
- alh3
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title abstract 12
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 title abstract 5
- 229910000091 aluminium hydride Inorganic materials 0.000 title abstract 5
- 239000003849 aromatic solvent Substances 0.000 title abstract 2
- 238000004821 distillation Methods 0.000 title 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract 3
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 abstract 2
- 229910010084 LiAlH4 Inorganic materials 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- 239000012280 lithium aluminium hydride Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Aluminium hydride is prepared in stable crystalline form by reacting AlCl3 with Li AlH4 using 1 mole AlCl3 to 4 moles LiAlH4 in solution in ether, giving an ether soln. of AlH3, and a ppte of LiCl which is then separated out. The solution is then mixed with an aromatic solvent esp. toluene in a proportion of 3:1 to the ether soln. and the soln. is distilled at reduced pressure, esp. 175-500 in Hg, at 50-85 (50-65) degrees C until only 8-10% of the mixt. is ether. The temp. is then increased to 90-100 degrees C to converts the AlH3 to a stable form, i.e. as 30-50 mu dia crystals, which are recovered. Used as a rocket propulsion fuel, AlH3 is more convenient to handle in crystalline form than as a soln. in ether, as a fine powder or as an agglomerate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7334979A FR2245569A1 (en) | 1973-10-01 | 1973-10-01 | Crystalline aluminium hydride prepn - by slow distillation of an ether/aromatic solvent soln |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7334979A FR2245569A1 (en) | 1973-10-01 | 1973-10-01 | Crystalline aluminium hydride prepn - by slow distillation of an ether/aromatic solvent soln |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| FR2245569A1 true FR2245569A1 (en) | 1975-04-25 |
Family
ID=9125742
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR7334979A Withdrawn FR2245569A1 (en) | 1973-10-01 | 1973-10-01 | Crystalline aluminium hydride prepn - by slow distillation of an ether/aromatic solvent soln |
Country Status (1)
| Country | Link |
|---|---|
| FR (1) | FR2245569A1 (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0650924A1 (en) * | 1993-10-27 | 1995-05-03 | Th. Goldschmidt AG | Process for the preparation of aluminium hydride (AlH3) by the reaction of magnesium hydride with aluminium halide |
| WO2000076913A1 (en) * | 1999-06-16 | 2000-12-21 | Sri International | Preparation of aluminum hydride polymorphs, particularly stabilized alpha-alh¿3? |
| RU2175637C2 (en) * | 1999-02-08 | 2001-11-10 | Российский Федеральный Ядерный Центр - Всероссийский Научно-Исследовательский Институт Экспериментальной Физики | Method of increasing thermal stability of aluminum hydride upon storage |
| RU2190571C2 (en) * | 1999-10-20 | 2002-10-10 | Самарский государственный технический университет | Method for storage of hydrogen under severe conditions |
| WO2013184616A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method for preparation of alane-etherate and alane |
| WO2013184617A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method of manufacturing alane including desolvation of an alane -etherate complex |
| WO2014058528A1 (en) | 2012-10-09 | 2014-04-17 | Intelligent Energy, Inc. | Method for preparation of crystalline alane using quaternary ammonium aluminum hydride |
| US9550672B2 (en) | 2012-06-05 | 2017-01-24 | Intelligent Energy Inc. | Method for preparation of an alane-etherate complex and alane |
| RU2648420C1 (en) * | 2017-04-18 | 2018-03-26 | Федеральное государственное унитарное предприятие "Центральный научно-исследовательский институт химии и механики" (ФГУП "ЦНИИХМ") | Method of producing alpha aluminium hydride |
-
1973
- 1973-10-01 FR FR7334979A patent/FR2245569A1/en not_active Withdrawn
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0650924A1 (en) * | 1993-10-27 | 1995-05-03 | Th. Goldschmidt AG | Process for the preparation of aluminium hydride (AlH3) by the reaction of magnesium hydride with aluminium halide |
| RU2175637C2 (en) * | 1999-02-08 | 2001-11-10 | Российский Федеральный Ядерный Центр - Всероссийский Научно-Исследовательский Институт Экспериментальной Физики | Method of increasing thermal stability of aluminum hydride upon storage |
| WO2000076913A1 (en) * | 1999-06-16 | 2000-12-21 | Sri International | Preparation of aluminum hydride polymorphs, particularly stabilized alpha-alh¿3? |
| RU2190571C2 (en) * | 1999-10-20 | 2002-10-10 | Самарский государственный технический университет | Method for storage of hydrogen under severe conditions |
| WO2013184616A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method for preparation of alane-etherate and alane |
| WO2013184617A1 (en) | 2012-06-05 | 2013-12-12 | Eveready Battery Company, Inc | Method of manufacturing alane including desolvation of an alane -etherate complex |
| US9550672B2 (en) | 2012-06-05 | 2017-01-24 | Intelligent Energy Inc. | Method for preparation of an alane-etherate complex and alane |
| WO2014058528A1 (en) | 2012-10-09 | 2014-04-17 | Intelligent Energy, Inc. | Method for preparation of crystalline alane using quaternary ammonium aluminum hydride |
| RU2648420C1 (en) * | 2017-04-18 | 2018-03-26 | Федеральное государственное унитарное предприятие "Центральный научно-исследовательский институт химии и механики" (ФГУП "ЦНИИХМ") | Method of producing alpha aluminium hydride |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| ST | Notification of lapse |