DE741779C - Process for the production of phenols from oils - Google Patents
Process for the production of phenols from oilsInfo
- Publication number
- DE741779C DE741779C DEM152824D DEM0152824D DE741779C DE 741779 C DE741779 C DE 741779C DE M152824 D DEM152824 D DE M152824D DE M0152824 D DEM0152824 D DE M0152824D DE 741779 C DE741779 C DE 741779C
- Authority
- DE
- Germany
- Prior art keywords
- oils
- phenols
- phenol
- production
- substances
- 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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Gewinnung von Phenolen aus ölen Es ist schon. vorgeschlagen worden, phenolhaltige Wässer in ;der Wärme, etwa bei 5o0 und darüber, und gegebenenfalls unter Druck, z. B. bei 2 bis 2o atii und 12o bis 2oo°, zur Behandlung von phenolhaltigen Ölen- o. dgl. zu ver«~enden. Dabei nehmen die ph:enolhaltigenWässer neban Nvenig Neutralöl noch wesentliche Mengen wertvoller, unter 23o° siedender Phenole aus den Ölen, Teeren o. @dgl. auf. Nachdem auf ,diese Weisse ihre Konzentration. an Phenoden erhöht worden ist, werden sie .durch Extraktion mit Benzol, M.ittelölfraktionen und ähnlichen Kohlenwasserstoffen, besonders aber mit rein organischen Estern, tlthern oder Ketonen, z. B. Butvlacetat, Isopropyläther o. rdgl., oder auf andere Art von den Phenolen befreit.Process for obtaining phenols from oils It is nice. suggested been, phenol-containing waters in; the heat, about 50 and above, and possibly under pressure, e.g. B. at 2 to 2o atii and 12o to 2oo °, for the treatment of phenol-containing To use oils or the like. The ph: enol-containing waters take neban Nvenig Neutral oil still contains substantial amounts of valuable phenols boiling below 23o ° from the Oils, tars or the like. on. After that, these white people get their concentration. on phenodes has been increased, they are .by extraction with benzene, middle oil fractions and similar hydrocarbons, but especially with purely organic esters, ether or ketones, e.g. B. Butvlacetat, isopropyl ether o. The like., Or in another type of freed the phenols.
Dieses Verfahren kann noch dadurch verbessert werden, daß,den phenolhaltigen Wässern, die zur Behandlung der phenolhaltigen Öle o. ,dä,l. dienen, die Phenälaufnahme begünsti@gende Stoffe, z. B. Alkohole, Ketone, Ester o. @dgl. zugesetzt werden, in welchem Falle man vorteilhaft auch bei gewöhnlicher und sogar tieferer Temperatur (z. B. bei etwa 20°) arbeiten kann.This process can be further improved in that, the phenol-containing Water used to treat oils containing phenol o., Dä, l. serve, the Phenäaufaufnahme Favorable substances, e.g. B. alcohols, ketones, esters o. @ The like. are added, in which case one is advantageous also at ordinary and even lower temperature (e.g. at about 20 °) can work.
Bei @diesexn Verfahren werden aber aus den Extraktionswässern Rohphenole gewonnen, die noch @Teutralöl enthalten. Erfindungsgemäß werden aus den phen,olhaltigen Wässern in Alkalilauge klar lösliche Phenote dadurch erzielt, daß man die Neutralöle durch eine Behandlung der Extraktionswässer mit geringen Mengen Benzin, Benzol, Butylaoetat oder anderen Neutralöllösungsmitteln abtrennt. Auf rdiese Weise wird dann inm weiteren Verlauf der P'henolgewinnwng aus den Extraktionswässern ein qualitativ hochwertiges, neutralölfreies Phenol erhalten, welches keine Wiederauflösung in Lauge im Verlauf der .weiteren Reinigung benötigt. Das zur Extraktion des Neutralöls aus den phenolhaltigen Wässern verwendete Lösungsmittel kann satzweise oder fortlaufend regeneriert «-enden, oder es kann, wenn z. B. Schwelbenzin als Lösemittel verwendet wird, ,das ölhaltige Benzin in eine Abtrei:beanlage für benzinbeladene Waschöle zurückgegeben werden.In @diesexn processes, however, the extraction water turns into crude phenols that still contain @teutral oil. According to the invention from the phen, olhaltigen Soaking in alkali lye produces clearly soluble phenotes by using the neutral oils by treating the extraction water with small amounts of gasoline, benzene, Separates butyl acetate or other neutral oil solvents. In this way will then in the further course of the phenol recovery from the extraction water a qualitative one high-quality, neutral oil-free phenol, which does not dissolve again in Lye required in the course of further cleaning. That for the extraction of the neutral oil Solvents used from the phenolic waters can be batchwise or continuously regenerated «-Ends, or it can, if z. B. Schwelbezin as a solvent is used, the oil-containing gasoline in a demolition plant for gasoline-laden Wash oils are returned.
Es kann auch bei diesem Verfahren ein Teil der wässerigen Flüssigkeit nach Abscheidung der Phenole und gegebenenfalls nach vollständiger oder teil-,veiser Entfernung der sonstigen (darin noch enthaltenen, z. B. aus dem Schwel- oder Hydrierprozeß stammenden wertvollen Stoffe, wie ILetone, den vorlaufenden phenolllaltigeu Wässern zugesetzt werden. Beispiel Eine Mittelölfraktion vom Siedebereich von i5o bis r95° aus der Schweltiog oberschlesischer Steinhohle wurde zunächst mit Schwelwasser aus dein Teichen Schwelprozeß durch Extraktion bei 85° entphenolt. Aus dem wässerigen Extrakt wurde .das Phenol finit Butyl!acetat ausgezogen und durch Destillation vom Butvlacetat getrennt. Die so gewonnetien, bis 230° siedenden Phenole lösten sich nur zu 93° in Lauge. 7'1, blieben als neutrale öle ungelöst.Part of the aqueous liquid can also be used in this process after separation of the phenols and, if necessary, after complete or partial, viscous Removal of the others (still contained therein, e.g. from the smoldering or hydrogenation process valuable substances originating from, such as clay, the leading phenollaltigeu waters can be added. Example A medium oil fraction with a boiling range from 150 to 95 ° the Schweltiog Upper Silesian stone cave was initially made with smoldering water your pond smoldering process is dephenolated by extraction at 85 °. From the watery Extract was extracted. The phenol finite butyl acetate and by distillation of the Butvlacetate separated. The phenols, boiling up to 230 °, dissolved in this way only 93 ° in lye. 7'1, remained undissolved as neutral oils.
Die gleiche Fraktion wurde in derselben Weise entplienolt. Das abgekühlte, an Phenolen angereicherte Schwelwasser wurde dann viermal reit je 20°/o seines Volumeils Petroläther vom Siedebereich d.o bis 8o° ausgeschüttelt. Darauf wurde .der Petroläther von der wässerigen Lösung geschieden, und aus der wässerigen Lösung wurden die Phenole niit Butylacetat in der gleichen Weise wie vorher gewonnen. Die P enole waren nunmehr in L e sIlich. Nach Abdampfung des au klar lös n Petrolätherextraktes blieb ein Öl zurück, das noch ungefähr 2o°/, Phenole enthielt.The same fraction was split up in the same way. The cooled smoldering water, enriched in phenols, was then extracted four times with 20% of its volume of petroleum ether from the boiling range do to 80 °. The petroleum ether was then separated from the aqueous solution, and the phenols with butyl acetate were obtained from the aqueous solution in the same manner as before. The P enols were now Silich in L e. After evaporation of the clear, dissolved petroleum ether extract, an oil remained which still contained about 20% phenols.
Man kann nach dem Verfahren gemäß der Erfindung auch Öle behandeln, die vorher mit schwach alkalischen Lösungen, z. B. von N a.#C 03, i\Ta H C 0;i, (N H4): C 03 von Tce rsä Uren befreit worden sind. Es werden dann reinere Phenole gewonnen.The process according to the invention can also be used to treat oils, the previously with weakly alkaline solutions, z. B. from N a. # C 03, i \ Ta H C 0; i, (N H4): C 03 have been freed from acidic acids. It then becomes purer phenols won.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEM152824D DE741779C (en) | 1940-11-14 | 1940-11-14 | Process for the production of phenols from oils |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEM152824D DE741779C (en) | 1940-11-14 | 1940-11-14 | Process for the production of phenols from oils |
Publications (1)
Publication Number | Publication Date |
---|---|
DE741779C true DE741779C (en) | 1944-04-25 |
Family
ID=7337113
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DEM152824D Expired DE741779C (en) | 1940-11-14 | 1940-11-14 | Process for the production of phenols from oils |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE741779C (en) |
-
1940
- 1940-11-14 DE DEM152824D patent/DE741779C/en not_active Expired
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