Claims
- 1. A process for the production of an alkali metal aluminum tetrahydride comprising pressure hydrogenating an alkali metal reactant and aluminum in an innocuous reaction medium at about 65.degree.-300.degree. C. and at least about 100-5,000 psi in the presence of an aluminate catalyst formed by heating sodium aluminum tetrachloride under hydrogen pressure in the presence of alkali metal and aluminum.
- 2. The process of claim 1 wherein said alkali metal is sodium or lithium.
- 3. The process of claim 2 wherein said alkali metal is sodium.
- 4. The process of claim 1 wherein said innocuous reaction medium is an ether.
- 5. The process of claim 4 wherein said ether is a polyether.
- 6. The process of claim 5 wherein said polyether is a diloweralkyl ether of an alkylene glycol.
- 7. The process of claim 6 wherein said diloweralkyl ether is a diloweralkyl ether of an ethylene glycol.
- 8. The process of claim 7 wherein said diloweralkyl ether of an ethylene glycol is the dimethyl ether of diethylene glycol.
- 9. The process of claim 1 wherein said reaction medium is a hydrocarbon.
- 10. The process of claim 9 wherein said hydrocarbon is toluene.
- 11. The process of claim 1 wherein said pressure hydrogenating is at about 750 to 2000 psi.
- 12. The process of claim 11 wherein said pressure hydrogenating is at about 900 to 1100 psi.
- 13. The process of claim 1 carried out at about 100.degree.-190.degree. C.
- 14. The process of claim 13 carried out at about 120.degree.-160.degree. C.
- 15. The process of claim 14 wherein said pressure hydrogenating is at about 1000 psi carried out at about 140.degree. C.
- 16. The process of claim 1 wherein said catalyst is formed in situ.
- 17. The process of claim 16 wherein sodium aluminum tetrachloride is present in the amount of about 1 to 15 mole parts per 100 gram-atom parts alkali metal reactant, to form the catalyst.
- 18. The process of claim 17 wherein sodium aluminum tetrachloride is present in the amount of about 2 to 5 mole parts per 100 gram-atom parts alkali metal reactant.
- 19. The process of claim 18 wherein said alkali metal reactant is sodium.
- 20. A semi-continuous process for the production of alkali metal aluminum tetrahydride, said process comprising the steps of:
- (a) pressure hydrogenating an alkali metal reactant with about a stoichiometric excess of aluminum in an innocuous reaction medium at about 65.degree.-300.degree. C. and at least about 100 to 5,000 psi in the presence of an aluminate catalyst formed by heating sodium aluminum tetrachloride under hydrogen pressure in the presence of alkali metal and aluminum;
- (b) withdrawing alkali metal aluminum tetrahydride product so as to leave an activated aluminum heel for recycle in a subsequent hydrogenating step;
- (c) adding alkali metal reactant and any additional aluminum required to make a reaction mixture containing about a stoichiometric excess of aluminum; and
- (d) pressure hydrogenating said reaction mixture and recovering product alkali metal aluminum tetrahydride.
- 21. The process of claim 20 wherein said stoichiometric excess is at least about 2 gram-atom parts aluminum per gram-atom part alkali metal reactant.
- 22. The process of claim 20 wherein said innocuous reaction medium is a diloweralkyl ether of an alkylene glycol.
- 23. The process of claim 22 wherein said diloweralkyl ether of an alkylene glycol is the dimethyl ether of ethylene glycol or the dimethyl ether of diethylene glycol.
- 24. The process of claim 20 wherein said catalyst in step (a) is formed in situ from about 1 to 15 mole parts NaAlCl.sub.4 per 100 gram-atom parts alkali metal reactant.
- 25. An active aluminum-containing aluminate liquid heel comprising a major portion of a reaction medium innocuous to pressure hydrogenation of alkali metal reactant and aluminum, and a minor portion of an aluminate catalyst species formed by heating an alkali metal reactant, aluminum, and NaAlCl.sub.4 at at least about 65.degree. C. under at least about 100 psig hydrogen pressure.
- 26. The process of claim 25 wherein the catalyst species is formed at at least about 100.degree. C. and 500 psig hydrogen pressure.
CROSS-REFERENCE
This application is a Continuation-in-Part of U.S. patent application Ser. No. 450,032, filed Dec. 15, 1982, now U.S. Pat. No. 4,528,176.
US Referenced Citations (5)
Foreign Referenced Citations (4)
Number |
Date |
Country |
1084700 |
Jul 1960 |
DEX |
1105167 |
Mar 1968 |
GBX |
1185707 |
Mar 1970 |
GBX |
186983 |
Oct 1966 |
SUX |
Non-Patent Literature Citations (2)
Entry |
Zakharkin et al., "Acad. of Sciences, USSR, Proceedings", vol. 145, Aug. 1962, pp. 656-658. |
Ashby et al., "Inorg. Chem.," vol. 2, No. 3, Jun. 1963, pp. 499-504. |
Continuation in Parts (1)
|
Number |
Date |
Country |
Parent |
450032 |
Dec 1982 |
|