DE489456C - Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues - Google Patents

Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues

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Publication number
DE489456C
DE489456C DEI30504D DEI0030504D DE489456C DE 489456 C DE489456 C DE 489456C DE I30504 D DEI30504 D DE I30504D DE I0030504 D DEI0030504 D DE I0030504D DE 489456 C DE489456 C DE 489456C
Authority
DE
Germany
Prior art keywords
pyridine
homologues
water
production
hydrogenation products
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
DEI30504D
Other languages
German (de)
Inventor
Dr Hans Spannagel
Eduard Tschunkur
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.)
IG Farbenindustrie AG
Original Assignee
IG Farbenindustrie AG
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 IG Farbenindustrie AG filed Critical IG Farbenindustrie AG
Priority to DEI30504D priority Critical patent/DE489456C/en
Application granted granted Critical
Publication of DE489456C publication Critical patent/DE489456C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D295/00Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
    • C07D295/02Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
    • C07D295/027Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pyridine Compounds (AREA)

Description

Verfahren zur Gewinnung von wasserfreien Reduktions- und Hydrierungsprodukten des Pyridins und seiner Homologen . Wasserhaltige Reduktions- und Hydrierungsprodukte des Pvridins und seiner Homologen lassen sich bekanntlich durch fraktionierte Destillation von Wasser n icht ganz befreien.Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues. Hydrous reduction and hydrogenation products It is known that pvridine and its homologues can be obtained by fractional distillation do not completely remove water.

Die Entwässerung dieser Basen. geschieht in der Technik deshalb durch Behandlung mit festen Ätzalkalien, ein Verfahren, das in der technischen Ausführung umständlich und kostspielig ist.The drainage of these bases. is therefore carried out in technology Treatment with solid caustic alkalis, a process that is in technical execution is cumbersome and expensive.

Es wurde nun gefunden, daß die Reduktions-und Hydrierungsprodukte des Pyridins und seiner Homologen durch Destillation vollkommen entwässert werden können, wenn man diesen wasserhaltigen Basen indifferente, mit Wasser nicht mischbare Stoffe, wie z. B. Benzol, Benzin oder Trichloräthylen, deren Siedepunkt in Mischungen mit Wasser unter dem Siedepunkt der wäßrigen Basen liegt, zusetzt.It has now been found that the reduction and hydrogenation products of pyridine and its homologues can be completely dehydrated by distillation can, if these water-containing bases are indifferent, immiscible with water Substances such as B. benzene, gasoline or trichlorethylene, their boiling point in mixtures with water is below the boiling point of the aqueous bases, adds.

Die Ausführung der Entwässerung kann in gewöhnlichen Destillatiqnsapparaten mit- oder ohne Kolonne nach dem Prinzip der kontinuierlichen oder diskontinuierlichen Destillation ausgeführt werden. Die hierbei zusammen mit Wasser abdestillierten Zusatzstoffe können nach Abtrennung des Wassers der Destillation kontinuierlich wieder zugeführt werden, wodurch die Mengen der Zusatzstoffe auf ein Mindestmaß beschränkt werden können.The drainage can be carried out in ordinary distillation apparatus with or without a column according to the principle of continuous or discontinuous Distillation can be carried out. The here distilled off together with water After the water has been separated off, additives can be added continuously by distillation be fed back, reducing the amounts of additives to a minimum can be restricted.

Die. Entwässerung von Pyridin selbst auf diesem Wege ist bekannt (vgl. die amerikanischen Patentschriften i 290 214 und 1416 2o6). Es war jedoch nicht vorauszusehen, daß die bekanntlich viel stärker zur Hydratbildung neigenden Hydrierungsprodukte des Pyridins, deren Basizität sogar so stark ist, daß sie Kohlensäure aus der Luft aufnehmen, auf diese einfache Weise sich entwässern lassen würden. Beispiel 5 ooo kg Piperidin mit 6o °!" Wassergehalt und i ooo kg Leichtbenzin werden in einer Destillierblase mit Kolonne' und Wasserabscheider zum Kochen erhitzt. Bei. etwa 32' Innentemperatur in der Blase destilliert ein Gemisch von Wasser und reinem Leichtbenzin über, das im Wasserabscheider derart getrennt wird, daß das Benzin wieder der Blase zugeführt wird, während das von Piperidin nahezu freie Wasser abläuft. Sobald 3 0001 Wasser abgetrennt sind, wird das Leichtbenzin vom Piperidin abdestilliert. In der Destillierblase bleiben i 9q.o kg wasserfreies Piperidin = etwa des Einsatzes.The. Dehydration of pyridine itself in this way is known (cf. American patents i 290 214 and 1416 2o6). However, it could not be foreseen that the hydrogenation products of pyridine, which are known to have a much stronger tendency to hydrate and whose basicity is so strong that they absorb carbonic acid from the air, could be dehydrated in this simple way. Example 5,000 kg of piperidine with 60 °! "Water content and 10,000 kg of light petrol are heated to the boil in a still with a column and water separator Water separator is separated in such a way that the gasoline is returned to the bladder, while the water, which is almost free from piperidine, runs off. As soon as 3,000 liters of water have been separated off, the light gasoline is distilled off from the piperidine. 9q.o kg of anhydrous piperidine = about of use.

Die genannten Zusatzstoffe können durch andere indifferente, mit Wasser nicht mischbare Stoffe mit Erfolg ersetzt werden, ebenfalls können die Mengen der Zusatzstoffe in weiten Grenzen schwanken.The additives mentioned can be indifferent to others, with water Immiscible substances can be successfully replaced, as can the quantities of Additives vary within wide limits.

Claims (1)

PATI:\ TA-; SPRUCH Verfahren zur Gewinnung von wasserfreien Reduktions- und I-Ivdrierungsprodukten des Pyridins und seiner Homologen durch fraktionierte Destillation, dadurch gekennzeichnet, daB man den zu entwässernden Basen mit Wasser nicht mischbare Stoffe, deren Siedepunkt in Mischungen mit Wasser unter dem Siedepunkt der wä.B-rigen Basen liegt. zusetzt.PATI: \ TA-; SPRUCH Process for the production of anhydrous reduction and I-Ivdrierungsprodukte of pyridine and its homologues by fractionated Distillation, characterized in that the bases to be dehydrated are mixed with water Immiscible substances whose boiling point in mixtures with water is below the boiling point of the aqueous bases. clogs.
DEI30504D 1927-03-03 1927-03-03 Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues Expired DE489456C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEI30504D DE489456C (en) 1927-03-03 1927-03-03 Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEI30504D DE489456C (en) 1927-03-03 1927-03-03 Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues

Publications (1)

Publication Number Publication Date
DE489456C true DE489456C (en) 1930-01-16

Family

ID=7187641

Family Applications (1)

Application Number Title Priority Date Filing Date
DEI30504D Expired DE489456C (en) 1927-03-03 1927-03-03 Process for the production of anhydrous reduction and hydrogenation products of pyridine and its homologues

Country Status (1)

Country Link
DE (1) DE489456C (en)

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