DE748377C - Process for the production of phenols from phenol-containing hydrocarbons or hydrocarbon-containing phenols - Google Patents

Process for the production of phenols from phenol-containing hydrocarbons or hydrocarbon-containing phenols

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Publication number
DE748377C
DE748377C DE1941748377D DE748377DD DE748377C DE 748377 C DE748377 C DE 748377C DE 1941748377 D DE1941748377 D DE 1941748377D DE 748377D D DE748377D D DE 748377DD DE 748377 C DE748377 C DE 748377C
Authority
DE
Germany
Prior art keywords
phenols
phenol
hydrocarbon
distillate
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
DE1941748377D
Other languages
German (de)
Inventor
Dr Alfred Dierichs
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 filed Critical
Application granted granted Critical
Publication of DE748377C publication Critical patent/DE748377C/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C37/76—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation by steam distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/005—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from products, waste products or side-products of processes, not directed to the production of phenols, by conversion or working-up
    • C07C37/007—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from products, waste products or side-products of processes, not directed to the production of phenols, by conversion or working-up from the tar industry

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Verfahren zur Gewinnung von Phenolen aus phenolhaltigen Kohlenwasserstoffen bzw. kohlenwasserstoffhaltigen Phenolen . Vorliegende Erfindung betrifft Verbesserungen in- der Gewinnung von Phenolen aus phenolhaltigen Kohlenwasserstoffen bzw. kohlenwasserstoffhaltigen Phenolen durch Wasserdampfdestillation. Es ist bekannt, daß- aus derartigen Gemischen die Anteile an eutralölen durch Wasserdampfdestillation entfernt werden können und daß hierbei ein praktisch reines Rohphenol zurückbleibt. Es besteht aber hierbei die Schwierigkeit, daß bei der Wasserdampfdestillation nicht Ar die N eutralöle übergehen, sondern in steigendem 'Maße auch Phenole.Process for the production of phenols from phenol-containing hydrocarbons or hydrocarbon-containing phenols. The present invention relates to improvements in the extraction of phenols from phenol-containing hydrocarbons or hydrocarbons Phenols by steam distillation. It is known that from such mixtures the proportions of eutral oils can be removed by steam distillation and that this leaves a practically pure crude phenol. But there is here the difficulty that Ar is not the neutral oils in steam distillation pass over, but increasingly also phenols.

Die Verbesserung gemäß vorliegender Erfindung besteht darin, daß man die wäßrige Schicht des Destillates, die im wesentlichen die übergegangenen Phenole enthält, in die Destillationshlase zurückführt. Besonders vorteilhaft arbeitet man in'der Weise, daß inan (las Destillat über die Destillationssäule in das Destillationsgefäß zurückleitet. Durch (las Berieseln del Destillationssäule mit dem wäßrigen Kondensat wird eine bessere Rektifikation erreicht. Ferner läßt rrian zweckmäßig die Kondensationsanlage so arbeiten, daß das Destillat möglichst heiß abgeschieden wird. Dadurch wird die Extraktionswirkung der wäßrigen Schicht besonders groß. Wenn nian in dieser Weise arbeitet, gelingt es, den Anteil an Phenol im Sumpf der Kolonne zu vergrößern. Das übergehende \Teütralöl enthält nur noch geringe Mengen an Phenolen. Sofern die Rohöle organische Basen enthalten, setzt man zweckmäßig etwas Säure, z. B. Schwefelsäure, zu, um die Basen zu binden und dadurch in der wäßrigen Phase zurückzuhalten.The improvement of the present invention is that one the aqueous layer of the distillate, which essentially contains the transferred phenols contains, returns to the distillation tube. One works particularly well in such a way that inan (read the distillate through the distillation column into the distillation vessel returns. The aqueous condensate was sprinkled through the distillation column a better rectification is achieved. Furthermore, rrian expediently leaves the condensation plant work so that the distillate is deposited as hot as possible. This will make the Extractive effect of the aqueous layer is particularly great. If nian in this way works, it is possible to increase the proportion of phenol in the bottom of the column. That Transient oil only contains small amounts of phenols. Unless the crude oils contain organic bases, it is expedient to use some acid, e.g. B. sulfuric acid, to to bind the bases and thereby retain them in the aqueous phase.

Beispiel ioo 1 einer Teerölfraktion vom Siedebereich i50 bis z95° und einen spez. Gewicht von 0,955, die 4.o % laugenlösliche Bestandteile enthält, wird mit io 1 Wasser versetzt und über eine mit Raschigringen gefüllte Kolonne destilliert. Das anfallende. zweckmäßig heiße Destillat wird einer Trennflasche zugeführt und der, wäßrige Anteil über die Kolonne zurückgeleitet. Wenn 63 101 überdestilliert sind, das noch geringe Mengen an laugenlöslichen Bestandteilen enthält!wird die Destillation unterbrochen. Das im Kolben zurückbleibende 01 besteht vorzugsweise aus Phenolen, die nur noch o,4 % laugenunlösliche Bestandteile enthalten.Example ioo 1 of a tar oil fraction from the boiling range i50 to z95 ° and a spec. Weight of 0.955, which contains 40 % lye-soluble constituents, is mixed with 10 l of water and distilled over a column filled with Raschig rings. The accruing. expediently hot distillate is fed to a separating bottle and the aqueous portion is returned via the column. When 63 101 has distilled over, which still contains small amounts of lye-soluble components! The distillation is interrupted. The oil remaining in the flask consists preferably of phenols which only contain 0.4% of lye-insoluble constituents.

Claims (3)

PATENTANSPRÜCHE: r. Verfahren zur Gewinnung voll Phenolen aus pltenolhaltigen Kohlenwasserstoften bzw. kohlenwasserstoffhaltigen Phenölen durch Wasserdampfdestillation, dadurch gekennzeichnet, daß man die wäßrige Schicht des Destillates in die Destillationsblase zurückführt. PATENT CLAIMS: r. Process for obtaining full phenols from pltenol-containing hydrocarbons or hydrocarbon-containing phen oils by steam distillation, characterized in that the aqueous layer of the distillate is returned to the still. 2. Verfahren nach Anspruch r, dadurch gekennzeichnet, daß man das Destillat über die Destillationssäule zurückleitet. 2. The method according to claim r, characterized in that the distillate is returned via the distillation column. 3. Verfahren nach Anspruch r und 2, dadurch gekennzeichnet, daß das Destillat 6e bei erhöhter Temperatur abgeschieden wird. Zur Abgrenzung des Anmeldungsgegenstandes vom Stand der Technik sind im Erteilungsverfahren keine Druckschriften in Betracht gezogen worden.3. The method according to claim r and 2, characterized in that the distillate 6e is deposited at an elevated temperature. To delimit the subject of the registration No publications from the state of the art are considered in the granting procedure been drawn.
DE1941748377D 1941-09-11 1941-09-11 Process for the production of phenols from phenol-containing hydrocarbons or hydrocarbon-containing phenols Expired DE748377C (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE748377T 1941-09-11

Publications (1)

Publication Number Publication Date
DE748377C true DE748377C (en) 1944-11-02

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ID=6648928

Family Applications (1)

Application Number Title Priority Date Filing Date
DE1941748377D Expired DE748377C (en) 1941-09-11 1941-09-11 Process for the production of phenols from phenol-containing hydrocarbons or hydrocarbon-containing phenols

Country Status (1)

Country Link
DE (1) DE748377C (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1110174B (en) * 1952-06-26 1961-07-06 California Research Corp Process for the production of hydrocarbon-free phenol
DE1125943B (en) * 1957-11-27 1962-03-22 Dr Rudolf Bemmann Process for removing neutral oil from phenolate liquors containing the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1110174B (en) * 1952-06-26 1961-07-06 California Research Corp Process for the production of hydrocarbon-free phenol
DE1125943B (en) * 1957-11-27 1962-03-22 Dr Rudolf Bemmann Process for removing neutral oil from phenolate liquors containing the same

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