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 homologuesInfo
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic 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
- C07D295/02—Heterocyclic 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
- C07D295/027—Heterocyclic 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)
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) |
-
1927
- 1927-03-03 DE DEI30504D patent/DE489456C/en not_active Expired
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