US3639104A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Preparation of magnesium aluminum hydride
Assignee: Ethyl Corp
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Filing: 1963-03-29
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Granted: 1972-02-01
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Expires: 1983-03-29
Abstract
Abstract 1. A method for the preparation of magnesium aluminum hydride which comprises reacting sodium aluminum hydride with an anhydrous magnesium halide in an ether as reaction solvent said ether being selected from the group consisting of unsubstituted alkyl ethers, diethylene glycol dialkyl ethers, and tetrahydrofuran mechanically separating the impure solid reaction products, separating magnesium aluminum hydride etherate from said reaction product by treatment with an ether as extractant for said etherate said ether being selected from the group consisting of unsubstituted alkyl ethers, diethylene glycol dialkyl ethers and tetrahydrofuran removing said extractant from the extract by evaporation thereof to dryness, removing the complexed ether by heating said etherate under reduced pressure to a temperature not in excess of 100* C. and recovering essentially ether-free magnesium aluminum hydride.
Inventors
- 👤 Eugene C Ashby
- 👤 Walter E Foster
- 👤 Horace E Redman
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 21:34
CPC Classifications
C; C01; C01B; C01B6/00; C01B6/24
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
124 words
A METHOD FOR THE PREPARATION OF MAGNESIUM ALUMINUM HYDRIDE WHICH COMPRISES REACTING SODIUM ALUMINUM HYRIDE WITH ANHYDROUS MAGNESIUM HALIDE IN AN ETHER AS REACTION SOLVENT SAID ETHER BEING SELECTED FROM THE GROUP CONSISTING OF UNSUBSTITUTED ALKYL ETHERS, DIETHYLENE GYLCOL DIALKYL ETHERS, AND TETRAHYDROFURAN MECHANICALLY SEPARATING THE IMPURE SOLID REACTION PRODUCTS, SEPARATING MAGNESIUM ALUMINUM HYDRIDE ETHERATE FROM SAID REACTION PRODUCT BY TREATMENT WITH AN ETHER AS EXTRACTANT FOR SAID ETHERATE SAID ETHER BEING SELECTED FROM THE GROUP CONSISTING OF UNSUBSTITUTED ALKYL ETHERS, DIETHYLENE GLYCOL DIALKYL EHTERS AND TETRAHYDROFURAN REMOVING SAID EXTRACTANT FROM THE EXTRACT BY EVAPORATION THEREOF TO DRYNESS, REMOVING THE COMPLEX ETHER BY HEATING SAID EHTERATE UNDER REDUCED PRESSURE TO A TEMPERATURE NOT IN EXCESS OF 100*C. AND RECOVERING ESSENTIALLY ETHER-FREE MAGNESIUM ALUMINUM HYDRIDE.
Claim 2
Independent Claim
124 words
A METHOD FOR THE PREPARATION OF MAGNESIUM ALUMINUM HYDRIDE WHICH COMPRISES REACTING SODIUM ALUMINUM HYRIDE WITH ANHYDROUS MAGNESIUM HALIDE IN AN ETHER AS REACTION SOLVENT SAID ETHER BEING SELECTED FROM THE GROUP CONSISTING OF UNSUBSTITUTED ALKYL ETHERS, DIETHYLENE GYLCOL DIALKYL ETHERS, AND TETRAHYDROFURAN MECHANICALLY SEPARATING THE IMPURE SOLID REACTION PRODUCTS, SEPARATING MAGNESIUM ALUMINUM HYDRIDE ETHERATE FROM SAID REACTION PRODUCT BY TREATMENT WITH AN ETHER AS EXTRACTANT FOR SAID ETHERATE SAID ETHER BEING SELECTED FROM THE GROUP CONSISTING OF UNSUBSTITUTED ALKYL ETHERS, DIETHYLENE GLYCOL DIALKYL EHTERS AND TETRAHYDROFURAN REMOVING SAID EXTRACTANT FROM THE EXTRACT BY EVAPORATION THEREOF TO DRYNESS, REMOVING THE COMPLEX ETHER BY HEATING SAID EHTERATE UNDER REDUCED PRESSURE TO A TEMPERATURE NOT IN EXCESS OF 100*C. AND RECOVERING ESSENTIALLY ETHER-FREE MAGNESIUM ALUMINUM HYDRIDE.
Claim 3
Dependent Claim
12 words
The method of claim 1 wherein the magnesium halide is magnesium chloride.
Claim 4
Dependent Claim
11 words
The method of claim 1 wherein the reaction solvent is tetrahydrofuran.
Claim 5
Dependent Claim
12 words
The method of claim 1 wherein the reaction solvent is dimethyl ether.
Claim 6
Dependent Claim
12 words
The method of claim 1 wherein the reaction solvent is diethyl ether.
Claim 7
Dependent Claim
11 words
The method of claim 1 wherein the extractant is diethyl ether.
Claim 8
Dependent Claim
11 words
The method of claim 1 wherein the extractant is dimethyl ether.
Claim 9
Dependent Claim
57 words
The method of claim 1 wherein the complexed ether is removed by heating the etherate under a reduced pressure of essentially 10 3 mm. of mercury for 18 to 30 hours at a temperature not in excess of 60* C. and then for 30 minutes to 2 hours at a temperature not in excess of 95* C.
Claim 10
Dependent Claim
133 words
A process for the preparation of magnesium aluminum hydride, which comprises intermixing sodium aluminum hydride with magnesium chloride in a reaction medium consisting of tetrahydrofuran to thereby react the sodium aluminum hydride with magnesium chloride to obtain a precipitate of magnesium aluminum hydride solvated with the reaction medium and sodium chloride, separating the precipitate from the reaction mixture, contacting the precipitate with a selective solvent, said solvent being a member selected from the group consisting of said reaction medium and alkyl ethers, thereby to separate the solvated magnesium aluminum hydride from the remaining constituents in the precipitate, recovering the separated solid magnesium aluminum hydride in its solid form, heating the solid solvated magnesium aluminum hydride to a temperature in the range of 60* to 100* C. to desolvate the solvated magnesium aluminum hydride.
Claim 11
Dependent Claim
133 words
A process for the preparation of magnesium aluminum hydride, which comprises intermixing sodium aluminum hydride with magnesium chloride in a reaction medium consisting of tetrahydrofuran to thereby react the sodium aluminum hydride with magnesium chloride to obtain a precipitate of magnesium aluminum hydride solvated with the reaction medium and sodium chloride, separating the precipitate from the reaction mixture, contacting the precipitate with a selective solvent, said solvent being a member selected from the group consisting of said reaction medium and alkyl ethers, thereby to separate the solvated magnesium aluminum hydride from the remaining constituents in the precipitate, recovering the separated solid magnesium aluminum hydride in its solid form, heating the solid solvated magnesium aluminum hydride to a temperature in the range of 60* to 100* C. to desolvate the solvated magnesium aluminum hydride.
Claim 12
Dependent Claim
141 words
A process for the preparation of magnesium aluminum hydride, which comprises intermixing sodium aluminum hydride with magnesium chloride in a reaction medium consisting of tetrahydrofuran, to thereby react the sodium aluminum hydride with magnesium chloride to obtain a precipitate of magnesium aluminum hydride solvated with the reaction medium and sodium chloride, separating the precipitate from the reaction mixture, contacting the precipitate with selective solvent, said solvent being a member selected from the group consisting of the members of said reaction medium and alkyl ethers, thereby to separate the solvated magnesium aluminum hydride from the remaining constituents in the precipitate, recovering the separated solvated magnesium aluminum hydride in its solid form, heating the solid solvated magnesium aluminum hydride to a temperature in the range of from the decomposition temperature of the solvate to 120* C. to desolvate the solvated magnesium aluminum hydride.
Claim 13
Dependent Claim
141 words
A process for the preparation of magnesium aluminum hydride, which comprises intermixing sodium aluminum hydride with magnesium chloride in a reaction medium consisting of tetrahydrofuran, to thereby react the sodium aluminum hydride with magnesium chloride to obtain a precipitate of magnesium aluminum hydride solvated with the reaction medium and sodium chloride, separating the precipitate from the reaction mixture, contacting the precipitate with selective solvent, said solvent being a member selected from the group consisting of the members of said reaction medium and alkyl ethers, thereby to separate the solvated magnesium aluminum hydride from the remaining constituents in the precipitate, recovering the separated solvated magnesium aluminum hydride in its solid form, heating the solid solvated magnesium aluminum hydride to a temperature in the range of from the decomposition temperature of the solvate to 120* C. to desolvate the solvated magnesium aluminum hydride.
References Cited (Backward Citations)
US3179490A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1975-01-31 | 1975-08-02 | 1976-02-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-01-31 | 1979-08-02 | 1980-02-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-01-31 | 1983-08-02 | 1984-02-01 | $7700.00 | Window Closed / Lapsed |