DE746350C - Process for the preparation of aqueous ammoniacal solutions - Google Patents

Process for the preparation of aqueous ammoniacal solutions

Info

Publication number
DE746350C
DE746350C DEO23952D DEO0023952D DE746350C DE 746350 C DE746350 C DE 746350C DE O23952 D DEO23952 D DE O23952D DE O0023952 D DEO0023952 D DE O0023952D DE 746350 C DE746350 C DE 746350C
Authority
DE
Germany
Prior art keywords
water
preparation
under pressure
aqueous ammoniacal
ammoniacal solutions
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
Application number
DEO23952D
Other languages
German (de)
Inventor
Dr-Ing Habil Gerhard Ruehl
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.)
Dr C Otto and Co GmbH
Original Assignee
Dr C Otto and Co 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
Application filed by Dr C Otto and Co GmbH filed Critical Dr C Otto and Co GmbH
Priority to DEO23952D priority Critical patent/DE746350C/en
Application granted granted Critical
Publication of DE746350C publication Critical patent/DE746350C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia
    • C01C1/10Separation of ammonia from ammonia liquors, e.g. gas liquors

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Physical Water Treatments (AREA)

Description

Verfahren zur Aufbereitung wäßriger ammoniakalischer Lösungen Der Erfindung liegt die Aufgabe zugrunde, bei der Aufbereitung von ammoniakalischen wäßrigen Lösungen, beispielsweise von Gaswässern, wie sie insbesondere bei der HochtemPeraturverkokung von Steinkohle und bei der Hydrierung von Brennstoffen anfallen, oder von Arnmoniakwasser, das beim sogenanuten indirekten Verfahren während der Reinigung anfällt, den Schwefekwa.sserstoff in möglichst konzentrierter Form zu gewinnen und außerdem die' Betriebskosten der Ammoniakreinigung der Gase soweit wie möglich herabzusetzen.Process for the preparation of aqueous ammoniacal solutions The The invention is based on the object in the processing of ammoniacal aqueous solutions, for example of gas waters, as they are in particular in the case of HochtemPeraturverkokung from hard coal and from the hydrogenation of fuels, or from ammonia water, The so-called indirect process occurs during cleaning, the hydrogen sulphide in the most concentrated form possible and also the 'operating costs of the Reduce ammonia purification of the gases as much as possible.

Es wurde bereits vorgeschlagen, die Ab- treibung .gasförmiger Säuren unter Druck mehrerer Atmosphären durchzuführen. Der Erfinder fand, daßeine besonders vorteilhafte ausschließliche Abtrennung flüchtiger Säuren aus -dem Ammoniakwasser bei Drucken oberhalb 5 atü erzielt wird.It has been proposed that waste expulsion .gasförmiger acids under pressure of several atmospheres to perform. The inventor found that a particularly advantageous exclusive separation of volatile acids from the ammonia water is achieved at pressures above 5 atmospheres.

Das genannte. Verfahren wird gemäß der Erfindung dadurch verbessert, daß Idas auf= zubereitende Rohwasser unter Druck einem Wärmeaustausch mit dem entgasten Wasser unterworfen :wird, bevor es in einem Röhrenofen unter Druck erhitzt wird.That said. The method is improved according to the invention by that Ida's on = raw water to be prepared under pressure a heat exchange with the degassed Subjected to water: is before it is heated under pressure in a tube furnace.

Durch diese Maßnahme wird ein Freiwerden gasförmiger Säuren aus dem Rohwasser im Wärmeaustauscher verhindert. Infolge des Wegfalls von Gasblasenbildung an den Wänden des Wärmeaustausch.ers wird der Wärmeaustausch zwischen entgastem Wasser und Rohwasser wesentlich erhöht, so daß die im Röhrenerhitzer aufz@ulvendende Wärmemenge geringer bemessen werden kann. Außerdem wird eine Korrosion der Wände des Wärmeaustauschers .durch die gasfö.r,migen, bekanntlich stark korrodierenden Säuren weitgehend vermieden.This measure will release gaseous acids from the Prevents raw water in the heat exchanger. As a result of the elimination of gas bubble formation on the walls of the Wärmeaustausch.ers the heat exchange between degassed Water and raw water increased significantly, so that the in the tube heater aufz @ ulvendende The amount of heat can be measured lower. There will also be corrosion of the walls of the heat exchanger through the gaseous, moderate, known to be highly corrosive Acids largely avoided.

Nach einer besonderen Durchführungsform des Verfahrens. ,der Erfindung wird das unter Druck entsäuerte Wasser zwecks Gewinnung des Ammoniaks in eine Fraktionierkolonne entspannt -und bei Normaldruck weiterverarbeitet. Hierdurch ist es möglich, ohne Wärmezufuhr in der Fraktionierkolonne das Ammoniak vollständig abzutrennen.According to a special form of implementation of the procedure. ,the invention the water, deacidified under pressure, is put into a fractionation column for the purpose of recovering the ammonia relaxed - and processed further at normal pressure. This is it is possible to completely remove the ammonia in the fractionating column without supplying heat to separate.

An Hand der beiliegenden Zeichnung, die eilt Schema der Abtreibevorricht:ung zeigt, wird derGang des Verfahrens näher erläutert: Das zu ent,g.asende Wasser wird mittels .der Pumpe i durch den Wärmeaustauscher 2 in den Röhrenofen 3 gedruckt, hier unter Druck hochgeheizt und über das Reduzierventil 4 in die unter Druck stehende Trennkolonne 5 entspannt. Bei einem Arbeitsdruck von ]ieispiels,weise 5 atii und einer Temperatur von 185°, hinter dem Reduzierventil gemessen, und einer mit Hilfe des Rückflußkühlers 6 eingestellten Kopftemperatur der Kolonne von 35°, entweicht durch das Entspannungsventil 7 ein Gemisch von Schwefelwasserstoff und Kohlendioxyd, .das praktisch frei von Ammoniak ist. Die .entsäuerte, ainmoniakalische Lösung wird Hinter dem Ventil 8 entspannt und tritt in die Fraktionierkolonne 9 ein. Aus dem Wasserdampf-.Ammoniak-Gemisch wird in dein Rüc:kfluß:kühler io ein Teil des Wasserdampfes niedergeschlagen. Die ammoniakreichen Dämpfe streichen durch den mit wäßrigen Alkali- bzw. Erdalhal?-lösungen beschickten Turm i i, in dem die letzten Spuren von H..S und CO.- entfernt werden, und anschließend durch das Aktivkohlefilter 12, das empyreuniatische Bestandteile aufnimmt. Die Dämpfe werden anschließend in 13 kondensiert. Von hier läuft, je nach den Arbeitsbedingungen, mehr oder weniger konzentriertes reines Amnioniak-Wasser ab. Gegebenenfalls kann man auch auf flüssiges Ammoniak arbeiten. Beide Stoffe können ohne weiteres zur Herstellung von Salpetersäure dienen. Das von 9 ablaufende heile entgaste Wasser gibt seine Wärme im Wärineattst.auscher 2 an das kalte P\-oliw:i;ser ab.The process of the process is explained in more detail on the basis of the accompanying drawing, which shows a quick diagram of the expulsion device: The water to be degassed is pressed into the tube furnace 3 by means of the pump i through the heat exchanger 2, here heated under pressure and expanded via the reducing valve 4 into the pressurized separating column 5. At a working pressure of] ie example, 5 atii and a temperature of 185 °, measured downstream of the reducing valve, and a top temperature of the column of 35 ° set with the aid of the reflux condenser 6, a mixture of hydrogen sulfide and carbon dioxide escapes through the expansion valve 7. which is practically free of ammonia. The deacidified, ammoniacal solution is depressurized downstream of the valve 8 and enters the fractionation column 9 . Part of the water vapor is precipitated from the water vapor / ammonia mixture in the return flow: cooler. The ammonia-rich vapors sweep through the tower ii charged with aqueous alkali or Erdalhal? Solutions, in which the last traces of H..S and CO.- are removed, and then through the activated charcoal filter 12, which absorbs empyreunistic constituents. The vapors are then condensed in 13. From here, depending on the working conditions, more or less concentrated pure amnioniac water drains off. If necessary, you can also work with liquid ammonia. Both substances can easily be used to produce nitric acid. The healthy degassed water draining off from 9 gives off its heat in the heat exchanger 2 to the cold water.

Claims (2)

PATENTANSPRÜCHE: i. Verfahren zur Aufbereitung wäßriger ammoniakalischer Lösungen, insbesondere Gaswasser, unter gleichzeitiger Befreiung des Wassers von gasförmigen Säuren bei erhöhtemDruck, dadurch ge@enn@e@chnet, daß das Rohwasser unter Druck einem Wärmeaustausch mit dem entgasten Wasser unterworfen wird. PATENT CLAIMS: i. Process for the preparation of aqueous ammoniacal Solutions, especially gas water, with simultaneous removal of the water from gaseous acids at increased pressure, so that the raw water is subjected to heat exchange with the degassed water under pressure. 2. Verfahren nach Anspruch i, dadurch gekennzeichnet, daß das unter Druck entsäuerte Wasser zwecks Gewinnung des .Ammoniaks in eine Fralitionierl-zolonne entspannt und bei Normaldruck weiterverarbeitet wird. Zur Abgrenzung des Anineldungsgegenstandes vom Stand der Technik sind im Erteilungs.verfabren folgende Druckschriften in Betracht gezogen worden: deutsche Patentschriften , . . . @\ r. 313 918, 326;3o, 61243z, 661 88i; britische Patentschriften \Tr. 33;J191.1 t1111 386642-, österreichische Patentschrift .. 1r. 3; 91o; Dr. W. Gluu.d »Handb. .d. Kolterei#" 1928, SS.154.2. The method according to claim i, characterized in that the water deacidified under pressure for the purpose of obtaining the .Ammoniaks is relaxed in a fralitionierl-zolonne and further processed at normal pressure. To distinguish the subject of the application from the state of the art, the following publications were considered in the issuing procedure: German patents,. . . @ \ r. 313 918, 326; 3o, 61243z, 661 88i; British patents \ Tr. 33; J191.1 t1111 386642-, Austrian patent specification .. 1r. 3; 91o; Dr. W. Gluu.d »Handb. .d. Kolterei # "1928, pp.154.
DEO23952D 1938-12-22 1938-12-22 Process for the preparation of aqueous ammoniacal solutions Expired DE746350C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEO23952D DE746350C (en) 1938-12-22 1938-12-22 Process for the preparation of aqueous ammoniacal solutions

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEO23952D DE746350C (en) 1938-12-22 1938-12-22 Process for the preparation of aqueous ammoniacal solutions

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE976733C (en) * 1953-12-01 1964-04-02 Otto & Co Gmbh Dr C Process for the treatment of gas water and similar solutions
DE3532390A1 (en) * 1984-09-12 1986-06-19 Carl Still Gmbh & Co Kg, 4350 Recklinghausen Process for treating waste water arising in coking or other coal upgrading processes
DE4002624C1 (en) * 1990-01-30 1991-11-28 Still Otto Gmbh, 4630 Bochum, De

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE313918C (en) *
AT37910B (en) * 1908-06-27 1909-07-10 Berlin Anhaltische Maschb Ag Device for removing ammonia from gas water.
GB191400337A (en) * 1914-01-06 1914-09-24 Rene Fabry Improvements in Continuous Stills for the Dissociation of Chemical Solutions by Heat.
DE326730C (en) * 1917-11-25 1920-10-04 C H Borrmann Process and apparatus for the continuous distillation of light oil from washing oil. like
GB386642A (en) * 1930-04-16 1933-01-19 Ets Barbet Apparatus for eliminating benzole from benzolic oils
DE612432C (en) * 1931-01-31 1935-06-11 Koppers Company Of Delaware Removal of tar acids from liquids
DE661881C (en) * 1936-06-29 1938-07-04 Koppers Gmbh Heinrich Process for removing acidic contaminants from ammonia water

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE313918C (en) *
AT37910B (en) * 1908-06-27 1909-07-10 Berlin Anhaltische Maschb Ag Device for removing ammonia from gas water.
GB191400337A (en) * 1914-01-06 1914-09-24 Rene Fabry Improvements in Continuous Stills for the Dissociation of Chemical Solutions by Heat.
DE326730C (en) * 1917-11-25 1920-10-04 C H Borrmann Process and apparatus for the continuous distillation of light oil from washing oil. like
GB386642A (en) * 1930-04-16 1933-01-19 Ets Barbet Apparatus for eliminating benzole from benzolic oils
DE612432C (en) * 1931-01-31 1935-06-11 Koppers Company Of Delaware Removal of tar acids from liquids
DE661881C (en) * 1936-06-29 1938-07-04 Koppers Gmbh Heinrich Process for removing acidic contaminants from ammonia water

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE976733C (en) * 1953-12-01 1964-04-02 Otto & Co Gmbh Dr C Process for the treatment of gas water and similar solutions
DE3532390A1 (en) * 1984-09-12 1986-06-19 Carl Still Gmbh & Co Kg, 4350 Recklinghausen Process for treating waste water arising in coking or other coal upgrading processes
DE4002624C1 (en) * 1990-01-30 1991-11-28 Still Otto Gmbh, 4630 Bochum, De

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