PL817B1 - Method of separating phenols from carbolic oil. - Google Patents

Method of separating phenols from carbolic oil. Download PDF

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Publication number
PL817B1
PL817B1 PL817A PL81722A PL817B1 PL 817 B1 PL817 B1 PL 817B1 PL 817 A PL817 A PL 817A PL 81722 A PL81722 A PL 81722A PL 817 B1 PL817 B1 PL 817B1
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PL
Poland
Prior art keywords
oil
water
temperature
extraction
oils
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Application number
PL817A
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Polish (pl)
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Publication of PL817B1 publication Critical patent/PL817B1/en

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Jest rzecza zinajna, -ze 'z olei, otrzyma¬ nych przezi sucha destylaicje bituminów i na¬ stepna ewentualnie redestylacje, wydziela sie kwasne skladinliiki w tych olejaJch zawarte, przy pomocy wodorotlenku sodowego, cza- Sieim przy pomocy mieszanin siarczanu rodo¬ wego i wodorotlenku wapniowego. Kwasne te oleje sa najczesciej fenolem i pochód- nenii fenolu.Niniejszy wynalazek umozliwia przepro¬ wadzenie ekstrakcji takich kwasnych olei przy :z;astioisowainiru o wiele tainsizegO' srodka i dlatego przedstawia znaczne' korzysci tech- natezme, sizezególinie wobec wysokiej ceny wodorotlenku sodowego.Doswiadczenia wykazaly, ze jezeli oleje takie zmieszac z woda w temperaturze po¬ wyzej temperatury krytycznej rozpuszCzal- niosci odnosnych kwasinych substancyj, za¬ wartych w oleju, to wówczas kwasne te sub¬ stancje dziela sie dokladnie po polowie mie¬ dzy olej i wode. Przy pomocy kilkakrotnie powtarzanej takiej ekstrakcji mozna z la¬ twoscia dojsc do tego punktu, w którym juz zawartosc kwasnych substancyj w oleju be¬ dzie minimalna, a praktycznie zadna. Przy stosowaniu zasady przeciwpradu mozna sto¬ sunkowo malemi ilosciiami wody w zupelnio- sci wyekstrahowac kwasnie skladniki! olejów.Woda ta, uzyta do ekstrakcji, po ostygnie¬ ciu wydziela czesciowo rozpuszczone w so¬ bie kwasne skladniki oleju. Celem wydoby¬ cia tych skladników z wody mozna je zpo- wrotem z wody wyekstrahowac w tempera¬ turze ponizej'temperatury krytycznej rozpu¬ szczalnosci olejem, który posiada bardzo rózny punkt wrzenia od tych kwasnych sub¬ stancyj, i nastepnie wydzielic je przez, frak-cjoiuowana deistykucje O rezultatach zasto¬ sowania niniejszej metody, moga dac poje¬ cie nastepujace przyklady: . Przyklad I.Tak zwany olej karbolowy, otrzymany jako, frakcja z mazi pogazowej wzglednie oleju sredniego, otrzymanego1 z mazii poga¬ zowej o ciezalrze wlaso. 0,964 przy 15° C a o zawartosci 25°/0 fenoli, oznaciziomych me¬ toda ekstralkcji lugiem1 sodowym, ekstraho¬ wano kilkakrotnie malemi ilosciami wody w temperaturze powyizej| 84° C, która to teimperaturla jest krytyczna wzajemnej roz- puszcizialinosici feinolu i wody. Po przeróbce jednego litra oleju fenolowego otrzymano 750 cm3 oleju, który zawieral 2,5% kwais- nych skladników, i 1250 cm3 wody, która iza^ wierala, przeliczajac na: pierwotna ilosc oleju karbolowego, 23% fenoli r 3,5% zasadowych zwiazków, t. zw. pirydyn. W tym wypadku stosowano pieciokrotna ekstrakcje w tempe raturze okolo 95°. Doswiadczenie to powtó¬ rzono na malym aparacie ekstrakcyjnym Kubdeirschkycego i przy pomocy znacznie miniejszej ilosci wody, bo 900 om3, otrzy¬ mano jako rezultat olej, zawierajacy li tylko 0,5% kwasnych skladników, a woda eks¬ trakcyjna po ostygnieciu wydzielala obficio olej, który byl surowym kwasem karbolo¬ wym z cala zaiwartosoia pirydyn z oleju pier¬ wotnego.Przyklad II.Surowy olej karbolowy o ciezarze wlasc. 0,954 przy 15° C a zawartosci feinioli 29% ekstrahowano na jednej kolumnie Ku- bier&chky'ego zapoimoca wody. Na piec li¬ ii ów oleju karbolowego zuzywano 5600 cm3 wody. Nastepnie otrzymany roztwór wjgdny po oichloidzieiniu do temperatury nizej 0,84° C eksitrahowano * na drugiej kolumnie lekka frakcja toluolowa, destylujaca calkowicie) do temperaitury 145°. Otrzymano z 250 cm3 to- luolu 395 cm3 mieszaniny tioluolu i fenioili, z których po oddzieleniu pirydyn znanetmi sposobami, otrzymano fenol surowy przez frakcjonowana destylacje.- Otrzymano fenolu przedestylowanego -129 cm3. Olej karbolowy pierwotny nie 'zawieral zmacziniejszych: ilo¬ sci kwasnych skladników a takze! i pirydyn.Ten sam rezultat otrzymalo sie przy ekstrak¬ cji w temperaturze 150° Cpod cisnieniem okolo 2,5 atm., jednak ilosc zuzytej do eks¬ trakcji wody wynosila znaicznie mniiej. Na¬ tomiast, jesli pierwsza ekstrakcje prOwadzOi- no w temperaturze nie o wiele wyzszej od 84° C, otrzymano jako pteirwsize frakcje eks¬ trakcji kwas karboiloiwy, który oprócz piry¬ dyn zawieral w glównej swej m&isie fenol.W ten spioisób zauwazono pewna moiznlosc frakcyjnej ekstrakcji surowego oleju karbo¬ lowego. PL PLThere is a unique thing that from the oils obtained by the dry distillation of bitumens and the possible gradual redistillation, the acidic constituents of these oils are separated, contained in these oils with sodium hydroxide, sometimes with mixtures of rhodium sulfate and calcium. These acidic oils are most often phenol and a derivative of phenol. The present invention makes it possible to extract such acid oils with: astioisowainir with a large amount of agent and therefore present considerable technical advantages, especially in relation to the high cost of sodium hydroxide. have shown that if such oils are mixed with water at a temperature above the critical solubility temperature of the respective acidic substances contained in the oil, the acidic substances are split exactly halfway between the oil and the water. By repeating such extraction several times it is easy to reach a point where the acidic substances in the oil are already minimal, if not practically non-existent. When the countercurrent principle is used, the ingredients can be extracted acidically with relatively small amounts of water! This extraction water, when it cools down, releases the partially dissolved acid components of the oil. In order to extract these constituents from the water, they can be extracted back from the water at a temperature below the critical solubility temperature with an oil that has a very different boiling point from these acidic substances, and then separated by a fraction. cjoated deistinguishing The results of the application of this method can be given by the following examples:. EXAMPLE 1 So-called carbolic oil, obtained as a fraction of gas fumes or middle oil, obtained from fumes with a weight of the same weight. 0.964 at 15 ° C and containing 25% phenols, determined by the method of extraction with sodium hydroxide, was extracted several times with small amounts of water at a temperature above | 84 ° C, which temperature is critical to the mutual dissolution of feinol and water. After processing one liter of phenolic oil, 750 cm3 of oil was obtained, containing 2.5% of acid components, and 1250 cm3 of water, which was consumed, converting to: the original amount of carbolic oil, 23% of phenols, and 3.5% of basic compounds , t. pyridine. In this case, five extractions at a temperature of about 95 ° were used. This experiment was repeated on a small Kubdeirschkyck extraction apparatus and with the help of a much smaller amount of water, 900 m3, an oil was obtained as a result, containing only 0.5% of acid components, and the extraction water, after cooling, gave off oil abundantly. which was crude carbolic acid with all the pyridine content of primary oil. Example 2: Crude carbolic oil with a weight of its own. 0.954 at 15 ° C and 29% feinolate contents were extracted on one Kubier & Chky column to keep water out. 5,600 cm 3 of water were used for the furnace of carbolic oil leaves. Then the obtained solution, after being cooled down to a temperature lower than 0.84 ° C, was extracted * on the second column with a light toluol fraction, distilling completely) to a temperature of 145 °. Prepared from 250 cm3 of toluol 395 cm3 of a mixture of thiolol and phenolyls, from which, after separation of pyridines by known methods, crude phenol was obtained by fractionated distillation. - Distilled phenol was obtained -129 cm3. Primary carbolic oil did not contain the following ingredients: amounts of acidic ingredients and also! and pyridines. The same result was obtained with the extraction at 150 ° C under a pressure of about 2.5 atm, but the amount of water used for extraction was significantly less. On the other hand, if the first extraction was carried out at a temperature not much higher than 84 ° C, the obtained fraction of the extraction was carboilievic acid, which, in addition to pyridines, contained mainly phenol in its substance. extraction of crude carbon oil. PL PL

Claims (1)

1. Zastrzezenie pat en t o w e. Sposób wydzielania fenoli i homologów fenoli z olejów, zawierajacych te sklaldniki, tern znamienny, ze prowadzi sie ekstrakcje kwasnych olejów zapomoca wody w tempe¬ raturze przynajmniej wyzszej, niz tempera¬ tura krytyczna roizpusiziczalnoisoi tego sklad¬ nika kwasnego oleju, który jest najnizszym czlonem szeregu homologów. Tadeusz Kuczynski. ZAKLGRAF.KOZIANSKICH W KRAKOWIE i PL PL1. Patent claim. A method of isolating phenols and phenol homologues from oils containing these components, characterized by the fact that acid oils are extracted by means of water at a temperature at least higher than the critical temperature of this acid component. oil, which is the lowest member of the series of homologues. Tadeusz Kuczynski. KOZIANSKI TRAINERS IN KRAKOW and PL PL
PL817A 1922-12-18 Method of separating phenols from carbolic oil. PL817B1 (en)

Publications (1)

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PL817B1 true PL817B1 (en) 1924-11-29

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