DE411732C - Process for the preparation of alkali metal amides - Google Patents
Process for the preparation of alkali metal amidesInfo
- Publication number
- DE411732C DE411732C DE1924E0030552 DEE0030552D DE411732C DE 411732 C DE411732 C DE 411732C DE 1924E0030552 DE1924E0030552 DE 1924E0030552 DE E0030552 D DEE0030552 D DE E0030552D DE 411732 C DE411732 C DE 411732C
- Authority
- DE
- Germany
- Prior art keywords
- sodium
- alkali metal
- ammonia
- catalyst
- amide
- 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.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
- C01B21/0923—Metal imides or amides
- C01B21/0926—Metal imides or amides of alkali metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Description
Die Erfindung betrifft die Herstellung von Alkalimetallamiden. Als Beispiel soll in der
nachstehenden Besenreibung die Herstellung von Natriumamid erläutert werden.
Es ist bekannt, daß Lösungen von Natrium, in verflüssigtem Ammoniak Natriumamid unter Freisetzung von Wasserstoff bilden.
Die Reaktion geht jedoch sehr langsam vor sich. Platin beschleunigt die Reaktion katalyrisch.
The invention relates to the production of alkali metal amides. The production of sodium amide is to be explained as an example in the description below.
It is known that solutions of sodium in liquefied ammonia form sodium amide with the release of hydrogen. However, the reaction is very slow. Platinum accelerates the reaction catalyrically.
Die vorliegende Erfindung besteht nun in einem Verfahren zur Herstellung von Alkalimetallamiden in Gegenwart von verflüssigtem Ammoniak, das ein Salz (ein Cyanid oder ein Jodid) gelöst enthält und in Gegenwart eines geeigneten Katalysators. Die Erfindung umfaßt weiterhin die Benutzung hochgekohlten Eisens oder kohlenstoffreichen Stahles als Katalysator. Das Amid kann entweder aus Alkalimetall, welches als solches zugesetzt wurde, oder aus Alkalimetall, das durch Elektrolyse aus einer Amalgamanode entsteht, hergestellt werden.The present invention now consists in a process for the preparation of alkali metal amides in the presence of liquefied ammonia containing a salt (a cyanide or an iodide) in solution and in the presence of a suitable catalyst. The invention further encompasses the use of high carbon Iron or high carbon steel as a catalyst. The amide can be made from either Alkali metal, which was added as such, or from alkali metal, which was obtained by electrolysis is made from an amalgamamode.
Die beiliegende Zeichnung zeigt schematisch zwei Ausführungsformen von Zellen zur Ausübung der Erfindung.The accompanying drawing shows schematically two embodiments of cells for Exercise of the invention.
In Abb. ι ist 1 die elektrolytische Zelle, mit Kathode 2 aus kohlenstofrreichem Stahl und einer ständig zu- und abgeführten Anode aus Natriumamalgam. 4 ist der Elek-In Fig. 1 is the electrolytic cell, with cathode 2 made of high-carbon steel and an anode that is constantly fed in and out from sodium amalgam. 4 is the elec-
trolyt, und 3 sind in den Elektrolyten eintauchende katalytisch^ Stahlscheiben. Der Elektrolyt tritt durch ein Rohr 5 in das Filter 6 über, wobei der Flüssigkeitsstand des Elektrolyten in der Zelle durch die Anordnung eines Wehrs oder Überfallrolirs stets der gleiche bleibt. Das Filter 6 mit Filterplatte 8, beispielsweise aus feinem Drahtgewebe, hält das gebildete Natriumamid zurück.trolyt, and 3 are catalytic steel disks immersed in the electrolyte. Of the Electrolyte passes through a tube 5 into the filter 6, the liquid level of the Electrolytes always in the cell through the arrangement of a weir or raid roll-over roll remains the same. The filter 6 with filter plate 8, for example made of fine wire mesh, holds back the sodium amide formed.
Der abtropfende Elektrolyt wird durch ein Rohr in den Behälter 7 gedrückt. 9 ist die Leitung für den Zutritt von flüssigem. Ammoniak. Das gewaschene Amid wird im geschmolzenen Zustande durch Rohr 10 ablaufen gelassen.The electrolyte that drips off is pressed into the container 7 through a pipe. 9 is the Line for the access of liquid. Ammonia. The washed amide is melted in the Conditions drained through pipe 10.
Die nachstehenden Beispiele zeigen mehrere Ausführungsformen der Erfindung.The following examples illustrate several embodiments of the invention.
Der Elektrolyt besteht aus einer Lösung von 50 Gewichtsteilen Natriumcyanid in 100 Gewichtsteilen verflüssigtem Ammoniak. Die | Anode besteht aus Natriumamalgam mit einem Gehalt von 0,05 Prozent Natrium. Das durch ; die Elektrolyse erzeugte Natrium wird schnell in Natriumamid umgewandelt, das in der Natriumcyanidlösung fast unlöslich ist und deshalb als ein weißer Schlamm auskristallisiert. Der suspendierte Schlamm wird kontinuierlich aus der Zelle entfernt, indem man frische Natriumcyanidlösung aus dem Reservoir 7 hinzutreten läßt. Wenn das Filter 6 gefüllt ist, wird der Abfluß zu einem zweiten. Filter (nicht gezeigt) abgelenkt. Die Flüssig· keit wird ausgetrieben, indem man den Druck in 6 auf geeignete Weise erhöht. Der Kuchen von Natriumamid wird dann von der Mutterlauge freigewaschen, indem man verflüssigtes, frisches Ammoniak durch Ventil 9 hinzutreten läßt. Die Waschlösungen werden gleichfalls in den Behälter 7 übergeführt., Das gewaschene Amid wird schließlich etwas über seinen Schmelzpunkt, bis etwa 1500 C, erhitzt und durch das Ventil 10 in Formen abgelassen. The electrolyte consists of a solution of 50 parts by weight of sodium cyanide in 100 parts by weight of liquefied ammonia. The | Anode consists of sodium amalgam with a sodium content of 0.05 percent. That through; Sodium produced by electrolysis is quickly converted to sodium amide, which is almost insoluble in the sodium cyanide solution and therefore crystallizes out as a white sludge. The suspended sludge is continuously removed from the cell by allowing fresh sodium cyanide solution from the reservoir 7 to enter. When the filter 6 is filled, the drain becomes a second one. Filter (not shown) deflected. The liquid is expelled by increasing the pressure in 6 in a suitable manner. The sodium amide cake is then washed free of the mother liquor by allowing liquefied fresh ammonia to enter through valve 9. The washing solutions are also transferred into the container 7. The washed amide is finally heated slightly above its melting point, to about 150 ° C., and discharged through the valve 10 into molds.
Eine Natriumlösung wird z. B. durch Elektrolyse einer Lösung von Natriumcyanid in verflüssigtem. Ammoniak mit einer Anode von Natriumamalgam hergestellt. Auch kann man metallisches Natrium, das auf irgendeinem bekannten Wege hergestellt wurde, in verflüssigtem Ammoniak auflösen. Natriumcyanid wird zu dieser Lösung hinzugefügt, dia man in ein Stahlgefäß bei einer Temperatur von 17 bis 300 C unter Druck einbringt. Auch andere katalytisch© Scheiben als solche aus Stahl können angewandt werden. Abb. 2 zeigt einen hierfür geeigneten Apparat.A sodium solution is e.g. B. by electrolysis of a solution of sodium cyanide in liquefied. Ammonia made with an anode of sodium amalgam. It is also possible to dissolve metallic sodium, which has been produced in any known way, in liquefied ammonia. Sodium cyanide is added to this solution, which is introduced into a steel vessel at a temperature of 17 to 30 ° C. under pressure. Catalytic disks other than steel can also be used. Fig. 2 shows an apparatus suitable for this.
Festes Natrium wird in das Gefäß 12 durch die Tür 13 eingebracht. Eine Lösung von Natriumcyanid in verflüssigtem Ammoniak wird in Gefäß 14 eingeführt. Geeignete Mengen sind ein Teil Natrium, auf drei Teile Natriumcyanid und zehn Teile Ammoniak, aber diese Mengen können innerhalb weiter Grenzen schwanken. Bei geeigneter Konzentration, bilden sich nach dem Mischen zwei Schichten, wovon die obere Schicht eine Lösung von Natrium in. Ammoniak und die untere eine Lösung von Natriumcyanid in flüssigem Ammoniak darstellt. Die Cyanidlösung läßt man durch Rohr 15 in das Gefäß 12 übertreten,· Beide Schichten stehen in Berührung mit den; Stahlwandungen des Gefäßes 12 und mitkatalytischen Scheiben 16. Der entwickelte Wasserstoff tritt zusammen mit Ammoniak durch Rohr 17 aus und werden voneinander getrennt. Das gebildete Amid wird abfiltriert,, die Lösung durch Rohn 18 in das Gefäß 14 übergeführt, das Amid gewaschen, geschmolzen und wie in Beispiel 1 in Formen abgelassen. An Stelle von Natriumcyanid als inertes, in Ammoniak gelöstes Salz kann man auch Natriumiodid zur Lösung im verflüssigten Ammoniak verwenden. In verflüssigtem Ammoniak schwer lösliche Salze, wie beispielsweise Natriumchlorid, sind weniger gut geeignet. go Solid sodium is introduced into the vessel 12 through the door 13. A solution of sodium cyanide in liquefied ammonia is introduced into vessel 14. Suitable amounts are one part sodium, three parts sodium cyanide and ten parts ammonia, but these amounts can vary within wide limits. With a suitable concentration, two layers form after mixing, of which the upper layer is a solution of sodium in ammonia and the lower layer is a solution of sodium cyanide in liquid ammonia. The cyanide solution is allowed to pass through tube 15 into the vessel 12. Both layers are in contact with the; Steel walls of the vessel 12 and with catalytic disks 16. The hydrogen evolved, together with ammonia, emerges through pipe 17 and are separated from one another. The amide formed is filtered off, the solution is transferred through the tube 18 into the vessel 14, the amide is washed, melted and, as in Example 1, drained into molds. Instead of sodium cyanide as the inert salt dissolved in ammonia, sodium iodide can also be used to dissolve in liquefied ammonia. Salts that are sparingly soluble in liquefied ammonia, such as sodium chloride, are less suitable. go
Claims (4)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB3087423A GB222718A (en) | 1923-12-08 | 1923-12-08 | Improvements in and relating to the manufacture of alkali metal amides |
Publications (1)
Publication Number | Publication Date |
---|---|
DE411732C true DE411732C (en) | 1925-04-04 |
Family
ID=10314470
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE1924E0030552 Expired DE411732C (en) | 1923-12-08 | 1924-04-01 | Process for the preparation of alkali metal amides |
Country Status (4)
Country | Link |
---|---|
DE (1) | DE411732C (en) |
FR (1) | FR589963A (en) |
GB (1) | GB222718A (en) |
NL (1) | NL16018C (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1133351B (en) * | 1959-07-22 | 1962-07-19 | Houilleres Bassin Du Nord | Process for the preparation of ammoniacal solutions of alkali metal amides by electrolysis of solutions of the alkali metal salts in liquid ammonia |
-
0
- NL NL16018D patent/NL16018C/xx active
-
1923
- 1923-12-08 GB GB3087423A patent/GB222718A/en not_active Expired
-
1924
- 1924-03-28 FR FR589963D patent/FR589963A/en not_active Expired
- 1924-04-01 DE DE1924E0030552 patent/DE411732C/en not_active Expired
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1133351B (en) * | 1959-07-22 | 1962-07-19 | Houilleres Bassin Du Nord | Process for the preparation of ammoniacal solutions of alkali metal amides by electrolysis of solutions of the alkali metal salts in liquid ammonia |
Also Published As
Publication number | Publication date |
---|---|
NL16018C (en) | |
GB222718A (en) | 1924-10-09 |
FR589963A (en) | 1925-06-09 |
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