US4051185A
Expired / Lapsed
US
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Process for the reclamation of alkali metal alkylamides
Assignee: Atomic Energy of Canada Ltd AECL
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Filing: 1976-02-10
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Granted: 1977-09-27
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Expires: 1996-02-10
Abstract
Abstract Alkali metal alkylamides, for example, potassium methylamide or mixtures of lithium and potassium methylamides, containing impurities may be purified by a novel process. The first step of the process comprises reacting the alkali metal alkylamides, in solution in methylamine, with ammonia to form the corresponding alkali metal amides which precipitate from solution while the impurities remain dissolved. The solid alkali metal amides are then separated from the solution, e.g., by filtration. The solution containing the impurities is distilled; and the distillate, comprised of methylamine containing some ammonia, is contacted with the alkali metal amides under reflux conditions and then the solution is rectified to remove ammonia. Under these conditions the alkali metal amides react with the methylamine to form a solution in methylamine of alkali metal methylamides freed of impurities. The solution is suitable for use as a catalyst for a deuterium enrichment process.
Inventors
- 👤 John Fraser Prescott
- 👤 Emerson Cecil Sanford
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 03:42
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/082; B; B01; B01J; B01J31/00; B01J31/02; B01J31/0234; B01J31/0235; B01J31/0252; B01J31/40; B01J31/4015; C01B21/087; C01B21/092; C01B21/0923; C01B21/0926; B01J2531/00; B01J2531/10; B01J2531/11; B01J2531/12; B01J2531/13; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
81 words
A process for reclaiming alkali metal alkylamide systems in purified form which comprises: adding ammonia to a solution in a primary alkylamine of an alkali metal alkylamide together with impurities, including N,N'-dialkylformamidine, and allowing reaction between the ammonia and said alkali metal alkylamide to occur; separating the alkali metal amide so obtained from the solution; and reacting said alkali metal amide with a primary alkylamine under conditions where NH 3 is removed to form alkali metal alkylamide free from said impurities.
Claim 2
Dependent Claim
12 words
A process as in claim 1, wherein the alkali metal comprises sodium.
Claim 3
Dependent Claim
12 words
A process as in claim 1, wherein the alkali metal comprises lithium.
Claim 4
Dependent Claim
12 words
A process as in claim 1, wherein the alkali metal comprises potassium.
Claim 5
Dependent Claim
35 words
A process as in claim 1, in which the starting material is an alkylamide of a mixture of alkali metals, and the product is an alkylamide of said mixture of alkali metals, in purified form.
Claim 6
Dependent Claim
110 words
A process as in claim 1, comprising the steps of: a. adding ammonia to a solution of potassium methylamide in methylamine, and allowing reaction between the ammonia and said potassium methylamide to occur, said solution including impurities which do not react with the ammonia; b. separating the potassium amide so obtained from the mother liquor which contains said impurities; c. distilling the mother liquor; and d. contacting the distillate, comprised of methylamine containing ammonia, with the separated potassium amide and allowing reaction between said methylamine and said potassium amide to occur under ammonia removal conditions, whereby a solution in methylamine of potassium methylamide, essentially freed of said impurities, is obtained.
Claim 7
Dependent Claim
124 words
A process as in claim 1, comprising the steps of: a. adding ammonia to a solution of mixed alkali metal methylamides in methylamine, and allowing reaction between the ammonia and said mixed alkali metal methylamides to occur, said solution including impurities which do not react with the ammonia; b. separating the mixture of alkali metal amides so obtained from the mother liquor containing said impurities; c. distilling the mother liquor; and d. contacting the distillate, comprised of methylamine containing ammonia, with the separated mixture of alkali metal amides and allowing reaction between said methylamine and said mixture of alkali metal amides to occur under ammonia removal conditions, whereby a solution in methylamine of mixed alkali metal methylamides, essentially freed of said impurities, is obtained.
Claim 8
Dependent Claim
33 words
A process as in claim 7, wherein the starting material is a mixture of lithium and potassium methylamides, and the final product is a mixture of lithium and potassium methylamides, in purified form.
Claim 9
Dependent Claim
160 words
A process as in claim 6, comprising the steps of: a. contacting a solution in methylamine of potassium methylamide and decomposition products thereof, in a reaction vessel, with an ammonia-rich solution of ammonia in methylamine, until a slurry of potassium amide in a solution of said decomposition products and excess ammonia in methylamine is formed; b. separating the potassium amide from said solution by filtration; c. subjecting the filtrate to fractional distillation; d. contacting the distillate, consisting of a dilute solution of ammonia in methylamine, with said recovered potassium amide, whereby a slurry is obtained; e. rectifying said slurry in a fractionating column, whereby there is obtained a solution of essentially pure potassium methylamide in methylamine and an overhead of ammonia with some methylamine; f. withdrawing from the top of said fractionating column an ammonia-rich solution of ammonia in methylamine, and recycling said solution to said reaction vessel; and g. recovering said solution of essentially pure potassium methylamide in methylamine.
Claim 10
Dependent Claim
176 words
A process as in claim 7, comprising the steps of: a. contacting a solution in methylamine of mixed alkali metal methylamides and decomposition products thereof, in a reaction vessel, with an ammonia-rich solution of ammonia in methylamine, until a slurry of a mixture of solid alkali metal amides in a solution of said decomposition products and excess ammonia in methylamine is formed; b. separating the mixture of alkali metal amides from said solution by filtration; c. subjecting the filtrate to fractional distillation; d. contacting the distillate, consisting of a dilute solution of ammonia in methylamine, with said mixture of alkali metal amides, whereby a slurry is obtained; e. rectifying said slurry in a fractionating column, whereby there is obtained a solution of essentially pure mixed alkali metal methylamides in methylamine, and an overhead of ammonia with some methylamine; f. withdrawing from the top of said fractionating column an ammonia-rich solution of ammonia in methylamine, and recycling said solution to said reaction vessel; and g. recovering said solution of essentially pure mixed alkali metal methylamides in methylamine.
Claim 11
Dependent Claim
33 words
A process as in claim 10, wherein the starting material is a mixture of lithium and potassium methylamides, and the final product is a mixture of lithium and potassium methylamides in purified form.
Claim 12
Dependent Claim
54 words
A process as in claim 9 wherein the solution of potassium methylamide in methylamine of starting step (a) is derived from a catalytic process for the enrichment of deuterium in hydrogen, and said product solution of essentially pure potassium methylamide in methylamine from step (e) is suitable for recycling to said deuterium enrichment process.
Claim 13
Dependent Claim
56 words
A process as in claim 10 wherein the solution of mixed alkali metal methylamides of starting step (a) is derived from a catalytic process for the enrichment of deuterium in hydrogen, and said product solution of essentially pure mixed alkali metal methylamides in methylamine from step (e) is suitable for recycling to said deuterium enrichment process.
Claim 14
Dependent Claim
30 words
A process as in claim 6 wherein the amount of ammonia added to the potassium methylamide solution is from 1 to 10 moles of ammonia per mole of potassium methylamide.
Claim 15
Dependent Claim
38 words
A process as in claim 8 wherein the amount of ammonia added to the solution of mixed lithium and potassium methylamides is from 1 to 10 moles of ammonia per mole of said mixed lithium and potassium methylamides.
Claim 16
Dependent Claim
20 words
A process as in claim 4 wherein the mole ratio of ammonia to potassium methylamide is from 2:1 to 5:1.
Claim 17
Dependent Claim
24 words
A process as in claim 15 wherein the mole ratio of ammonia to said mixed lithium and potassium methylamides is from 2:1 to 5:1.
References Cited (Backward Citations)
CA552779A
Cited
US2612436A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-09-26 | 1981-03-28 | 1981-09-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-09-26 | 1985-03-28 | 1985-09-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-09-26 | 1989-03-28 | 1989-09-27 | $7700.00 | Window Closed / Lapsed |