DE301279C - - Google Patents

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Publication number
DE301279C
DE301279C DENDAT301279D DE301279DC DE301279C DE 301279 C DE301279 C DE 301279C DE NDAT301279 D DENDAT301279 D DE NDAT301279D DE 301279D C DE301279D C DE 301279DC DE 301279 C DE301279 C DE 301279C
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DE
Germany
Prior art keywords
autoclave
carbonic acid
ammonia
compressor
urea
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DENDAT301279D
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German (de)
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Publication of DE301279C publication Critical patent/DE301279C/de
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/04—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds from carbon dioxide and ammonia

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

AUSGEGEBEN AM 26. JANUAR 1922ISSUED ON JANUARY 26, 1922

KLASSE 12 ο GRUPPECLASS 12 ο GROUP

Es wurde gefunden, daß die Darstellung von Harnstoff aus Kohlensäure und Aiumö^ niak in einfacher Weise gelingt, wenn man das Gemisch der beiden Gase mittels Kompressors in einen Autoklaven drückt und die entstandene Schmelze, gegebenenfalls unter Zufuhr weiterer Wärme, genügend lange bei der für die Umwandlung von Ammoniumcarbaraat in Harnstoff geeigneten Temperatur hält. Dieses Verfahren wird dadurch besonders wertvoll, daß man mittels desselben kontinuierlich arbeiten kann, ohne daß wie bisher eine Abscheidung des unveränderten Ammoniumcarbamats in fester oder flüssiger Form erforderlich ist, indem man das bei der Entspannung der im Autoklaven enthaltenen Schmelze erhaltene Ammoniakkohlensäuregasgemisch unmittelbar durch den Kompressor in den Autoklaven zurückkomprimiert.It has been found that the preparation of urea from carbonic acid and Aiumö ^ niak succeeds in a simple way if one presses the mixture of the two gases into an autoclave by means of a compressor and the resulting melt, if necessary with the addition of further heat, for a long enough time the temperature suitable for the conversion of ammonium carbarate into urea holds. This process becomes particularly valuable in that it can be used continuously can work without a deposition of the unchanged ammonium carbamate as before in solid or liquid form is required by doing that during relaxation the ammonia-carbonic acid gas mixture obtained in the melt in the autoclave directly by the compressor compressed back into the autoclave.

Man verfährt z. B. in der Weise, daß man ein geeignetes, zweckmäßig etwas feuchtes Gemisch von Kohlensäure und Ammoniak mittels eines vorgewärmten Kompressors in einen Autoklaven drückt und die erhalteneOne proceeds z. B. in such a way that you have a suitable, appropriately something damp Mixture of carbonic acid and ammonia by means of a preheated compressor in an autoclave and the obtained

a5 Schmelze z. B. 2 Stunden auf 135° hält. Dann wird an einem Bodenventil langsam1 entspannt in einen Destillierapparat, z. B. eine Kolonne, in welcher teils durch die Eigenwärme der Schmelze, teils durch unten zugeführte Wärme das unveränderte Ausgangsmaterial als Ammoniak-Kohlensäure-Gasgemisch ausgetrieben wird, während unten fertige Harnstofflösung praktisch frei von Ammonsalizen abläuft. Das aus der zweckmäßig mit einem Dephlegmator versehenen Kolonne oben entweichende Gemisch von Ammoniak und Kohlensäure wird unmittelbar von dem vorgewärmten Kompressor angesaugt und in den Autoklaven hineinkomprimiert. Um das durch Harnstoffbildung verschwundene Ausgangsmaterial zu ersetzen, kann man entweder frische Kohlensäure und Ammoniak getrennt oder zusammen in den Autoklaven drücken oder noch einfacher in den oberen Teil der Kolonne eine wäßrige Lösung von Ammon- *5 carbamat oder -carbonat einfließen lassen, welche in einem besonderen Gefäß aus Kohlensäure und Ammoniak hergestellt werden kann, wobei dann auch die Verwendung von unreiner Kohlensäure möglich ist. Die Höhe des Wassergehaltes in dem vom Kompressor zurückzuführenden Ammoniak-KohTensäure-Gemisch läßt sich durch Einhaltung entsprechender Temperatur am Dephlegmatorausgang regeln, z.B. wählt man eine solche von 6o°. a 5 melt z. B. holds 2 hours at 135 °. Then 1 is slowly relaxed at a bottom valve in a still, z. B. a column in which the unchanged starting material is driven out as an ammonia-carbonic acid gas mixture partly by the intrinsic heat of the melt, partly by the heat supplied below, while the urea solution below runs practically free of ammonium salts. The mixture of ammonia and carbonic acid escaping from the top of the column, which is expediently provided with a dephlegmator, is sucked in directly by the preheated compressor and compressed into the autoclave. To replace the starting material that has disappeared due to the formation of urea, you can either press fresh carbonic acid and ammonia separately or together into the autoclave or, even more simply, let an aqueous solution of ammonium carbamate or carbonate flow into the upper part of the column, which in one Special vessel can be made from carbonic acid and ammonia, in which case the use of impure carbonic acid is also possible. The level of the water content in the ammonia-carbonic acid mixture to be fed back from the compressor can be regulated by maintaining the appropriate temperature at the dephlegmator outlet, for example a temperature of 60 ° is chosen.

Die Entspannung kann auch, um Kompressionsarbeit zu sparen, erst auf einen Zwischendruck, z. B. 10 Atm., erfolgen, wobei ein Teil des Kohlensäure-Ammoniak-Gemisches abdestilliert und unmittelbar z. B. der zweiten Stufe des Kompressors zugeführt wird, während der Rest nach der vollständigen Entspannung in der Kolonne verdampft und der ersten Stufe des Kompressors zugeleitet wird.In order to save compression work, the relaxation can only be done with an intermediate pressure, z. B. 10 atm., With part of the carbonic acid-ammonia mixture distilled off and immediately z. B. is fed to the second stage of the compressor while the rest evaporates after complete expansion in the column and the first Stage of the compressor is fed.

Claims (2)

Patent-An Sprüche: Patent-to sayings: ι . Verfahren zur Darstellung von Harnstoff, dadurch gekennzeichnet, daß man ein Gemisch von Kohlensäure und Ammoniak mittels Kompressors in einen Autoklaven drückt und die entstandene Schmelze, gegebenenfalls unter Zufuhrι. Process for the preparation of urea, characterized in that a mixture of carbonic acid and ammonia is placed in an autoclave by means of a compressor presses and the resulting melt, optionally with supply weiterer Wärme, genügend lange bei der für die Umwandlung von Aimmoniuimcarbamat in..Harnstoff,.geeigneten Temperatur halt.further heat, long enough for the conversion of ammonium carbamate in .. urea, .suitable temperature stop. 2. Ausführungsform des unter ι geVerfahrens, darin bekennzeichneten 2. Embodiment of the method under ι, identified therein stehend, daß man zum Zwecke kontinuierlichen Arbeitens das bei der Entspannung der im Autoklaven enthaltenen Schmelze erhaltene Ammoniak-Kohlensäure-Gemisch durch den Kompressor in den Autoklaven zurückkomprimiert.standing that for the purpose of continuous work one can do that with relaxation the ammonia-carbonic acid mixture obtained in the melt contained in the autoclave compressed back into the autoclave by the compressor.
DENDAT301279D 1916-08-09 Active DE301279C (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE145060X 1916-08-09

Publications (1)

Publication Number Publication Date
DE301279C true DE301279C (en)

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ID=5670562

Family Applications (1)

Application Number Title Priority Date Filing Date
DENDAT301279D Active DE301279C (en) 1916-08-09

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DE (1) DE301279C (en)
GB (1) GB145060A (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL259135A (en) * 1959-12-31 1900-01-01

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Publication number Publication date
GB145060A (en) 1921-05-19

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