DE492427C - Process for the production of oxygen-containing organic compounds - Google Patents

Process for the production of oxygen-containing organic compounds

Info

Publication number
DE492427C
DE492427C DEB112217D DEB0112217D DE492427C DE 492427 C DE492427 C DE 492427C DE B112217 D DEB112217 D DE B112217D DE B0112217 D DEB0112217 D DE B0112217D DE 492427 C DE492427 C DE 492427C
Authority
DE
Germany
Prior art keywords
water
organic compounds
oxygen
containing organic
production
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
DEB112217D
Other languages
German (de)
Inventor
Dr Marlin Luther
Dr Rudolf Wietzel
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 DEB112217D priority Critical patent/DE492427C/en
Application granted granted Critical
Publication of DE492427C publication Critical patent/DE492427C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/02Monohydroxylic acyclic alcohols
    • C07C31/04Methanol

Description

Verfahren zur Gewinnung von sauerstoffhaltigen organischen Verbindungen Im Patent 479 $29 ist ein Verfahren beschrieben, welches gestattet, die durch katalytische Hydrogenisation von Oxyden des Kohlenstoffs neben Methylalkohol @erhältlichen wasserhaltigen Gemische sauerstoffhaltiger organischer Verbindungen durch fraktionierte Destillation in einzelne Bestandteile zu zerlegen, indem man zuvor die Hauptmenge des Wassers aus dem Gemisch entfernt.Process for the production of oxygen-containing organic compounds The patent 479 $ 29 describes a process which allows the catalytic Hydrogenization of oxides of carbon in addition to methyl alcohol @ available hydrous Mixtures of oxygen-containing organic compounds by fractional distillation to be broken down into individual components, by first taking the bulk of the water removed from the mixture.

Es wurde nun gefunden, daß man auf sehr einfache Weise eine weitgehende Abtrennung des Wassers ,aus den genannten Gemischen erzielen kann, wenn man sie der -Ti!efkühlung unterwirft, so daß sich das Wasser in fester oder halbfester Form abscheidet. Mit dein Wasser zusammen scheiden sich hierbei im allgemeinen noch organischeVerblndungen ab:.It has now been found that one can, in a very simple manner, achieve an extensive Separation of the water from the mixtures mentioned can be achieved if you use them the -Ti! ef! subcooling, so that the water in solid or semi-solid form separates. Organic compounds are generally separated with your water away:.

Bei hohem Gehalt des Gemisches an Methylalkohol ist ein vorheriges Abdestillieren der Hauptmenge des letzteren zweckmäßig, unter Umständen sogar erforderlich, da man sonst sehr tief kühlen muß, weil größere Mengen Methylalkohol das Ausfrieren des Wassers erschweren. Beispiel Ein Rohprodukt, das bei der katalytischen Hydrierung eines aus 3oq% Kohlenoxyd und 709 Wasserstoff bestehenden Gasnsches bei ¢20° und Zoo Atm. Druck mittels eignes aus r 5 Teilen Kaliumbichronla,t, ¢ Teilen Zinkoxyd und 2 Teilen Kupferoxyd hergestellten Kontakts erhalten wurde, wird von der Hauptmenge des Methylalkohols durch Destillation oder Ausschütteln mi;t Wasser befreit. Der ölige Rückstand, der noch-etwa 2o0o 'Wasser enthält und ein spezifisches Gewicht von 0,86o besitzt, wird mittels Kohlensäureschnees abgekühlt und von dem, ausfallenden, hauptsächlich aus Wasser und Methylalkohol bestehenden Kristallbrei abgenutscht. In dem erhaltenen Filtrat, das etwa 750,"o des vorgenannten- öligen Rückstandes ausmacht und dessen spezifisches Gewicht nunmehr 0,823 beträgt, .sind jetzt nur noch geringe Mengen Wasser vorhanden; ein einfaches Destillieren genügt, um dien im Rohöl vorhandenen Isobutyl:alkohol (bei den oben angegebenen Arbeitsbedilngungen über 2o% des Rohproduktes) und daneben auch noch andere organische sauerstoffhäl'tilge Stoffe praktisch wasserfrei zu gewilnxien.If the mixture contains a high amount of methyl alcohol, it is advisable to distill off the bulk of the latter beforehand, and may even be necessary, since otherwise very deep cooling is required because larger amounts of methyl alcohol make it difficult for the water to freeze out. Example A crude product that is produced in the catalytic hydrogenation of a gas consisting of 30% carbon oxide and 70% hydrogen at 20 ° and zoo atm. Pressure obtained by means of a contact prepared from r 5 parts of potassium bichronla, t, [parts of zinc oxide and 2 parts of copper oxide, is freed from the bulk of the methyl alcohol by distillation or shaking with water. The oily residue, which still contains about 2o0 'of water and has a specific gravity of 0.86o, is cooled by means of carbon dioxide snow and sucked off the precipitating crystal pulp, consisting mainly of water and methyl alcohol. In the resulting filtrate, which makes up about 750. "O of the aforementioned oily residue and whose specific gravity is now 0.823, only small amounts of water are now present; a simple distillation is sufficient to remove the isobutyl alcohol present in the crude oil (with the above-mentioned Arbeitsbedilngungen over 20% of the crude product) and also other organic oxygen-containing substances to make practically anhydrous.

Die infolge :geringer Beimengungen oft gelblich gefärbte Isobutylalkoholfraktyon wird unter Zugabe von wenig metallischem Natrium oder auch von Pottasche rekdfm!ert. Es wird dann ein wasserheller, fast i ooprozentiger Isobutylalkohol gewonnen.The isobutyl alcohol fractyon, which is often yellowish in color as a result of minor admixtures is refined with the addition of a little metallic sodium or potash. A water-white, almost 100% isobutyl alcohol is then obtained.

Fügt man zu dem abzukühlenden Öl noch geeignete andere Stoffe, wie Benzol oder :aüssige schweflige Säure, hinzu, so tritt die Bildurig des Kristallbreies bedeutend leichter ein.If you add other suitable substances to the oil to be cooled, such as Benzene, or: external sulphurous acid, is added, and the image of the crystal pulp appears significantly easier.

An Stelle der geschilderten ArbiextsWesie kann man auch in der Weisse verfahren, .daß man das Rohprodukt fraktioniert und die bei 75 bis ioo° übergehende Fraktion, die aus einem Gemisch von Methylalkohol, Walsex, Isobutylalkohol und höher säjedenden Stoen besteht, das. sich durch gewälmlvcha Destillation nur mit großer Mühe und erst nach wiederholter Destillation trennen läßt, in der oben angegebenen Weise durch Tiefkühlung von der Hauptmasse des Wassers befreit und auf reinen Isobutylalkohol, wie oben angegeben, weiterverarbeitet.Instead of the described ArbiextsWesie you can also use the white procedure, .that the crude product is fractionated and that which passes over at 75 to 100 ° Fraction made up of a mixture of methyl alcohol, whale sex, isobutyl alcohol and above säjedenden Stoen consists, which can only be achieved by distillation with large Difficulty and only after repeated distillation can separate in the above Way freed from the bulk of the water by freezing and on pure isobutyl alcohol, further processed as stated above.

Claims (1)

PATENTANSPRUC73 Ausführungsform des Verfahrens des Hauptpatents 479 829, dadurch gekennzeichnet, daß das bei der katalytischen Hydrierung der Kohlenoxyde erhaltene Gemisch zur Entfernung des Wassers so tief gekühlt wird, daß :such das Wasser, gegebenenfalls zusammen mit organischen Verbindungen, in fester oder halbfester Form ausscheidet.PATENT CLAIM73 Embodiment of the process of main patent 479 829, characterized in that the mixture obtained in the catalytic hydrogenation of the carbon oxides is cooled so deeply to remove the water that: such as the water, optionally together with organic compounds, precipitates in solid or semi-solid form.
DEB112217D 1924-01-03 1924-01-03 Process for the production of oxygen-containing organic compounds Expired DE492427C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEB112217D DE492427C (en) 1924-01-03 1924-01-03 Process for the production of oxygen-containing organic compounds

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEB112217D DE492427C (en) 1924-01-03 1924-01-03 Process for the production of oxygen-containing organic compounds

Publications (1)

Publication Number Publication Date
DE492427C true DE492427C (en) 1930-02-24

Family

ID=6993148

Family Applications (1)

Application Number Title Priority Date Filing Date
DEB112217D Expired DE492427C (en) 1924-01-03 1924-01-03 Process for the production of oxygen-containing organic compounds

Country Status (1)

Country Link
DE (1) DE492427C (en)

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