DE1036223B - Process for the recovery of water enriched in heavy water in the course of ammonia synthesis using an isotope exchange between ammonia and hydrogen gas - Google Patents

Process for the recovery of water enriched in heavy water in the course of ammonia synthesis using an isotope exchange between ammonia and hydrogen gas

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Publication number
DE1036223B
DE1036223B DEU4070A DEU0004070A DE1036223B DE 1036223 B DE1036223 B DE 1036223B DE U4070 A DEU4070 A DE U4070A DE U0004070 A DEU0004070 A DE U0004070A DE 1036223 B DE1036223 B DE 1036223B
Authority
DE
Germany
Prior art keywords
ammonia
water
enriched
deuterium
isotope
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.)
Pending
Application number
DEU4070A
Other languages
German (de)
Inventor
Dipl-Ing Hans Hesky
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ThyssenKrupp Industrial Solutions AG
Original Assignee
Uhde GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to BE560103D priority Critical patent/BE560103A/xx
Application filed by Uhde GmbH filed Critical Uhde GmbH
Priority to DEU4070A priority patent/DE1036223B/en
Priority to GB24844/57A priority patent/GB870452A/en
Priority to FR1180973D priority patent/FR1180973A/en
Publication of DE1036223B publication Critical patent/DE1036223B/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B5/00—Water
    • C01B5/02—Heavy water; Preparation by chemical reaction of hydrogen isotopes or their compounds, e.g. 4ND3 + 7O2 ---> 4NO2 + 6D2O, 2D2 + O2 ---> 2D2O
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/04—Preparation of ammonia by synthesis in the gas phase
    • C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
    • C01C1/0488—Processes integrated with preparations of other compounds, e.g. methanol, urea or with processes for power generation
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Zur Anreicherung bzw. Gewinnung von schwerem Wasser im Zuge der Ammoniaksynthese sind eine Reihe von Verfahren bekannt, bei denen das zur Ammoniaksynthese erforderliche Wasserstoffgas auf seinem Wege zur Synthese zum Isotopenaustausch mit Wasser gebracht und derart das Wasser laufend an Deuteriumhydroxyd angereichert wird.For the enrichment or extraction of heavy water in the course of the ammonia synthesis are one Number of processes known in which the hydrogen gas required for ammonia synthesis brought its way to synthesis to isotopic exchange with water and so the water running is enriched in deuterium hydroxide.

Bei diesem Verfahren liegt die Gleichgewichtskonstante im Isotopenaustauscher relativ niedrig, und das in die Syntheseanlage eingeführte Synthesegas nimmt noch einen erheblichen Teil des Deuteriums mit.In this process, the equilibrium constant in the isotope exchanger is relatively low, and that Synthesis gas introduced into the synthesis plant still takes a considerable part of the deuterium with it.

Es ist auch bekannt, daß ein Isotopenaustausch zwischen Wasserstoffgas und Ammoniak möglich ist.It is also known that isotope exchange between hydrogen gas and ammonia is possible.

Die Erfindung macht Gebrauch von dieser Art des Isotopenaustausches und besteht darin, den Ausgangswasserstoff mit einem Teil des aus ihm erzeugten Ammoniaks zum Isotopenaustausch zu bringen und das derart an Deuteriumverbindungen angereicherte Ammoniak unter Wasserbildung, z. B. katalytisch zu Stickoxyd und Wasser, zu verbrennen.The invention makes use of this type of isotope exchange and consists in the starting hydrogen to bring to isotopic exchange with part of the ammonia produced from it and the ammonia enriched in this way in deuterium compounds with water formation, e.g. B. catalytically too Nitric oxide and water to burn.

Durch dieses Verfahren wird der höhere Konzentrationsunterschied zwischen den beiden zum Isotopenaustausch herangezogenen Phasen nutzbar gemacht und damit eine wesentlich höhere Ausbeute an mit schwerem Wasser angereichertem Wasser als bei den bekannten Verfahren erzielt.By doing this, the higher concentration difference between the two becomes an isotope exchange used phases made usable and thus a much higher yield water enriched with heavy water than achieved with the known methods.

Dadurch, daß das Ammoniak in der Syntheseanlage aus dem am Kopf der Isotopenaustauschkolonne abgezogenen Wasserstoff erzeugt wird, entspricht die Konzentration des Ammoniaks an Deuteriumverbindungen zwangläufig der Deuteriumkonzentration dieses Wasserstoffes, so daß die Ammoniaksynthese hier eine analoge Wirkung ausübt wie der Rücklaufkondensator bei Rektifikationskolonnen. Es kann also eine quantitative Deuteriumauswaschung in der Isotopenaustauschkolonne erzielt werden, so daß das in der Syntheseanlage erzeugte Ammoniak praktisch deuteriumfrei ist.Because the ammonia in the synthesis plant is withdrawn from the isotope exchange column at the top Hydrogen is generated, the concentration of ammonia corresponds to deuterium compounds inevitably the deuterium concentration of this hydrogen, so that the ammonia synthesis here has an effect similar to that of the reflux condenser in rectification columns. So it can be a quantitative deuterium leaching can be achieved in the isotope exchange column, so that in the The ammonia produced by the synthesis plant is practically free of deuterium.

Das bei der katalytischen Verbrennung des an Deuteriumverbindungen angereicherten Ammoniaks zu Stickoxyd und Wasser gewonnene, an schwerem Wasser angereicherte Wasser wird zweckmäßig einer Hochkonzentrationsstufe zugeführt. Das dort anfallende, an Deuteriumhydroxyd und -oxyd verarmte Gehalt an diesen Deuteriumverbindungen aufweist, als natürliches Wasser in die Anlage zur Erzeugung des natürliches Wasser, in die Anlage zur Erzeugung des Ausgangswasserstoffs zurückgeführt. Durch Anwendung des Isotopenaustauschs zwischen Ammoniak und Ausgangswasserstoff liegt die Gleichgewichtskonstante im Tsotopenaustauscher wesentlich höher als bei den bisher bekannten Anlagen, die mit dem Isotopenaustausch zwischen Wasserstoffgas und natürlichem Wasser arbeiten. Dadurch ergeben sich zwischen denThat in the catalytic combustion of ammonia enriched in deuterium compounds Water enriched in heavy water and obtained to nitrogen oxide and water is expediently one High concentration level fed. The accumulated there, depleted in deuterium hydroxide and oxide Has content of these deuterium compounds, as natural water in the plant for the production of the natural water, fed back into the plant for the production of the starting hydrogen. By application the isotope exchange between ammonia and starting hydrogen is the equilibrium constant in the isotope exchanger is significantly higher than in the previously known systems that deal with isotope exchange work between hydrogen gas and natural water. This results in between the

Verfahren
zur Gewinnung an schwerem Wasserprocedure
for the extraction of heavy water

angereicherten Wassersenriched water

im Zuge der Ammoniaksynthese unter Anwendung eines Isotopenaustauschesin the course of ammonia synthesis using an isotope exchange

zwischen Ammoniak und Wasserstoffgasbetween ammonia and hydrogen gas

Anmelder:Applicant:

Friedrich Uhde G.m.b.H.,
Dortmund, Deggingstr. 10-12Friedrich Uhde GmbH,
Dortmund, Deggingstrasse. 10-12

Dipl.-Ing. Hans Hesky, Dortmund,
ist als Erfinder genannt wordenDipl.-Ing. Hans Hesky, Dortmund,
has been named as the inventor

beiden Phasen höhere Konzentrationsunterschiede und die damit verbundenen Vorteile.higher concentration differences in both phases and the associated advantages.

Ein weiterer Vorteil des erfindungsgemäßen Verfahrens besteht darin, daß das Ammoniak in der Isotopenaustauschkolonne eventuell im Wasserstoff vorhandenen, für den Synthesekontakt schädlichen Wasserdampf entfernt, so daß das Synthesegas im Gegensatz zu der bisherigen Handhabung vor dem Ammoniakofen direkt in den Synthesekreislauf aufgegeben werden kann.Another advantage of the process according to the invention is that the ammonia in the isotope exchange column Any water vapor which may be present in the hydrogen and which is harmful to the synthesis contact removed, so that the synthesis gas in contrast to the previous handling before the ammonia furnace can be fed directly into the synthesis cycle.

Der Isotopenaustausch zwischen Ammoniak und Wasserstoff kann in der Gasphase erfolgen. Besonders zweckmäßig ist jedoch der Isotopenaustausch zwischen flüssigem Ammoniak und Wasserstoffgas in einem Kontaktbett oder mit Hilfe einer in der Flüssigkeit suspendierten Kontaktsubstanz, z. B. Platin.The isotope exchange between ammonia and hydrogen can take place in the gas phase. Particularly however, the isotope exchange between liquid ammonia and hydrogen gas in a contact bed or with the aid of a contact substance suspended in the liquid, e.g. B. platinum.

Setzt man beim Arbeiten mit Kontaktsuspension in den Austritt des an Deuterium angereicherten Ammoniaks aus dem Isotopenaustauscher ein Filter od. dgl. ein, so ist es möglich, die Kontaktsubstanz dauernd praktisch verlustfrei im Isotopenaustauscher umzuwälzen. When working with contact suspension, place in the outlet of the deuterium-enriched ammonia a filter or the like from the isotope exchanger, so it is possible to keep the contact substance permanently to circulate practically without loss in the isotope exchanger.

Die Zeichnung zeigt ein Schemabild einer AnlageThe drawing shows a schematic diagram of a plant

zur Durchführung des erfindungsgemäßen Verfahrens.for carrying out the method according to the invention.

Mit 1 ist eine beliebige Anlage zur Erzeugung vonWith 1 any system for the production of

Wasserstoff bezeichnet, der über die Leitung 2 Wasser zugeleitet wird. Das aus der Anlage 1 kommende Wasserstoffgas gelangt über die Leitung 3 in den Isotopenaustauscher 4 und von dort völlig verarmt an Deuterium, mit Stickstoff aus Leitung 8 vermischt, über die Leitung 5 in die Syntheseanlage 6. Von demDenotes hydrogen, which is fed via line 2 to water. The one coming from Appendix 1 Hydrogen gas reaches the isotope exchanger 4 via line 3 and from there it is completely depleted Deuterium, mixed with nitrogen from line 8, via line 5 into the synthesis plant 6. From the

809 597/500809 597/500

in der Synthese erzeugten Ammoniak wird ein Teil über die Leitung 7 in den Isotopenaustauscher zurückgeführt und nimmt dort Deuterium, z. B. in Form von H2ND, auf. Das derart angereicherte Ammoniak gelangt über die Leitung 9 in eine Verbrennungskammer 10, wo es zu Stickoxyd und mit schwerem Wasser angereichertem Wasser verbrannt wird. Das angereicherte Wasser gelangt über die Leitung 11 beispielsweise in eine Hochkonzentrationsanlage 12, wobei zweckmäßig das verarmte Wasser über die Leitung 13 in die Leitung 2 zurückgeführt wird, falls es noch an Deuteriumhydroxyd reicher ist als natürliches Wasser, während hochprozentiges schweres Wasser über die mit D2O bezeichnete Leitung aus der Anlage 12 abgezogen wird. igPart of the ammonia produced in the synthesis is returned to the isotope exchanger via line 7, where it takes deuterium, e.g. B. in the form of H 2 ND. The ammonia enriched in this way reaches a combustion chamber 10 via line 9, where it is burned to form nitrogen oxide and water enriched with heavy water. The enriched water passes via line 11, for example, into a high-concentration system 12, whereby the impoverished water is expediently returned via line 13 to line 2 if it is still richer in deuterium hydroxide than natural water, while high-percentage heavy water via the D 2 O designated line is withdrawn from the system 12. ig

Selbstverständlich ist es möglich, die Hochkonzentrationsanlage in Wegfall kommen zu lassen und an schwerem Wasser angereichertes Wasser unmittelbar aus der Leitung 11 zu entnehmen. Unter Umständen kann auch die Rückführung des verarmten Wassers über die Leitung 13 in die Leitung 2 entfallen.Of course, it is possible to leave the high-concentration system to be omitted and to arrive to remove heavy water enriched water directly from the line 11. In certain circumstances the return of the depleted water via line 13 into line 2 can also be omitted.

Bei Verwendung einer mit dem flüssigen Ammoniak umlaufenden Kontaktsubstanz kann am Ammoniakaustritt der Isotopenaustauschkolonne eine Abtrennvorrichtung 14 für die Kontaktsubstanz vorgesehen werden, die durch die Leitung 15 am Kopf der Isotopenaustauschkolonne in die Leitung 7 zurückgegeben wird.If a contact substance circulating with the liquid ammonia is used, there may be an outlet at the ammonia outlet the isotope exchange column, a separation device 14 is provided for the contact substance are returned to line 7 through line 15 at the top of the isotope exchange column will.

Claims (7)

Patentansprüche:Patent claims: 1. Verfahren zur Gewinnung an schwerem Wasser angereicherten Wassers im Zuge der Ammoniaksynthese unter Anwendung eines Isotopenaustauschers zwischen Ammoniak und Wasser- 3g stoffgas, dadurch gekennzeichnet, daß der Ausgangswasserstoff mit einem Teil des aus ihm erzeugten Ammoniaks zum Isotopenaustausch gebracht und das derart an Deuterium angereicherte Ammoniak unter Wasserbildung verbrannt wird.1. Process for the extraction of heavy water enriched water in the course of the ammonia synthesis using an isotope exchanger between ammonia and hydrogen 3g substance gas, characterized in that the starting hydrogen isotopically exchanged with part of the ammonia produced from it and enriched in this way in deuterium Ammonia is burned to form water. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das an Deuterium angereicherte Ammoniak katalytisch zu Stickoxyd und Wasser verbrannt wird.2. The method according to claim 1, characterized in that the enriched in deuterium Ammonia is catalytically burned to nitrogen oxide and water. 3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das durch die Verbrennung gewonnene, an Deuterium angereicherte Wasser einer Hochkonzentrationsstufe zugeführt wird.3. The method according to claim 1 or 2, characterized in that by the combustion recovered, deuterium-enriched water is fed to a high concentration stage. 4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß das in der Hochkonzentrationsstufe anfallende, an Deuterium verarmte Wasser in die Anlage zur Erzeugung des Ausgangswasserstoffes zurückgeführt wird.4. The method according to claim 3, characterized in that in the high concentration stage accumulating, deuterium-depleted water in the plant for the production of the starting hydrogen is returned. 5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der Isotopenaustausch zwischen flüssigem Ammoniak und Wasserstoffgas in Gegenwart einer Kontaktsubstanz erfolgt. 5. The method according to any one of claims 1 to 4, characterized in that the isotope exchange takes place between liquid ammonia and hydrogen gas in the presence of a contact substance. 6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß der Isotopenaustausch zwischen Ammoniak und Wasserstoff mittels einer Suspension einer Kontaktsubstanz in der Flüssigkeit erfolgt.6. The method according to claim 5, characterized in that the isotope exchange between ammonia and hydrogen takes place by means of a suspension of a contact substance in the liquid. 7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß am Ammoniakauslaß des Isotopenaustauschers die Katalysatorsubstanz abgefiltert und vorzugsweise in den Isotopenaustauscher zurückgeführt wird.7. The method according to claim 6, characterized in that the ammonia outlet of the isotope exchanger the catalyst substance is filtered off and preferably returned to the isotope exchanger will. In Betracht gezogene Druckschriften:
USA.-Patentschrift Nr. 2 690 379.Considered publications:
U.S. Patent No. 2,690,379. Hierzu 1 Blatt Zeichnungen1 sheet of drawings © 809 597/500 8.58© 809 597/500 8.58
DEU4070A 1956-08-17 1956-08-17 Process for the recovery of water enriched in heavy water in the course of ammonia synthesis using an isotope exchange between ammonia and hydrogen gas Pending DE1036223B (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BE560103D BE560103A (en) 1956-08-17
DEU4070A DE1036223B (en) 1956-08-17 1956-08-17 Process for the recovery of water enriched in heavy water in the course of ammonia synthesis using an isotope exchange between ammonia and hydrogen gas
GB24844/57A GB870452A (en) 1956-08-17 1957-08-07 Combined process for the production of water enriched with deuterium and the synthesis of ammonia
FR1180973D FR1180973A (en) 1956-08-17 1957-08-08 Process for enriching or obtaining heavy water during the synthesis of ammonia with isotope exchange between ammonia and hydrogen

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEU4070A DE1036223B (en) 1956-08-17 1956-08-17 Process for the recovery of water enriched in heavy water in the course of ammonia synthesis using an isotope exchange between ammonia and hydrogen gas

Publications (1)

Publication Number Publication Date
DE1036223B true DE1036223B (en) 1958-08-14

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Country Status (4)

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BE (1) BE560103A (en)
DE (1) DE1036223B (en)
FR (1) FR1180973A (en)
GB (1) GB870452A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1145585B (en) * 1959-11-18 1963-03-21 Basf Ag Process for the production of heavy hydrogen during the ammonia synthesis
DE1237546B (en) * 1959-03-13 1967-03-30 Air Liquide Process for obtaining water enriched with deuterium

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE581674A (en) * 1958-08-13
CN113526526A (en) * 2021-07-12 2021-10-22 苏州大学 Preparation method of deuterated ammonia and deuterated reaction taking deuterated ammonia as deuterium source to participate

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2690379A (en) * 1942-11-21 1954-09-28 Harold C Urey Process for production of deuterium oxide as a source of deuterium

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2690379A (en) * 1942-11-21 1954-09-28 Harold C Urey Process for production of deuterium oxide as a source of deuterium

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1237546B (en) * 1959-03-13 1967-03-30 Air Liquide Process for obtaining water enriched with deuterium
DE1145585B (en) * 1959-11-18 1963-03-21 Basf Ag Process for the production of heavy hydrogen during the ammonia synthesis

Also Published As

Publication number Publication date
GB870452A (en) 1961-06-14
BE560103A (en)
FR1180973A (en) 1959-06-10

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