Crude condensate

The KAL CON Environmental Services (a division of Kalkaska Constrnction Services, Inc.) thermal desorption process is an ex situ treatment technology that removes hydrocarbon contamination from soil. This process has been used to treat soils contaminated with gasoline, jet fuel, diesel fuel, kerosene, crude oil, and crude condensate. 

Fifty grams of powdered sulfur are introduced into the flask and heated to 150 °C in an oil bath under the hood while a moderately rapid stream (about 5 bubbles/sec) of dry chlorine is led over the molten sulfur. The crude orange-red product distills rapidly into the receiver. The chlorination requires about two hours and is stopped when only a very small amount of sulfur remains in the reaction flask. About 5-8g of sulfur are added to the crude condensate to combine with the excess of dissolved chlorine a redistillation yields over 90% of the dark yellow chloride boiling at 137-140°C. Large amounts of low-boiling materials must be distilled again from a little sulfur. To obtain a pure product, the material may be fractionated once more or distilled in vacuo b.p. 29-30°C (12mm). 

The crude condensation product is extracted successively with (a) light petroleum, (b) dry benzene and (c) dry chloroform, the first solvent removing any unchanged o-cresol. 

Isomeride (A).—The chloroform extract (c) of the foregoing crude condensation product on concentration and cooling gives a red solid which after many crystallisations from chloroform yields well-defined, transparent, colourless, oblique prisms, decomposing at 197° to 198° C. 

The crude condensation product is a dark semi-solid product which leaves an insoluble green solid after extraction with carbon tetrachloride. 

When the benzene mother-liquors from the compound described above are evaporated under 20 mm. pressure, a black viscous tar remains. This is extracted with chloroform and the extract added to the original chloroform extract of the crude condensation product. Concentration of the mixture yields a pink crystalline material three recrystallisations from chloroform giving colourless compact crystals, decomposing at 213° to 214° C. The complex is slightly more soluble in hot chloroform than in the cold solvent, and dissolves readily in alcohol or acetone. 

Dimethyl-4-carbethoxy-2-cyclohexen-l-one and 3,5-di-methyl-2-cyclohexen-l-one have always been prepared from acetaldehyde and acetoacetic ester through the Knoevenagel condensation.2 The keto ester has previously been obtained by selective saponification and decarboxylation methods which have involved heating the crude condensation product with water at 140° 2 3 or with sodium ethoxide in alcohol.3 The ketone has been obtained from the same condensation product by prolonged refluxing in 20% sulfuric acid.2-4 6... 

Vinylcyclopropane 24 (1.1 g, 2.91 mmol) was distilled under vacuum (0.5 Torr) through a tube heated to 610°C. The pyrolysate was collected in a trap cooled to — 78 C, and the trap contents were transferred to a flask and the solvent evaporated to give 1.06 g (96%) of the crude condensate, which was purified by chromatography on neutral alumina (activity grade 111) with hexane as eluant to give 25 as a mixture of C8 epimers (8a/8 2 1). 

In a subsequent modification pure, hexa-O-acetylipecoside was readily obtained by acetylation of the crude condensation product of dopamine with secologanin followed by column chromatography over silica gel (14). 

According to Wallace and Goodeve, the ClgO formed as described above may be purified by passing the crude condensate first over PgOg and then over precipitated but not heated 1 0 to remove any traces of unreacted Clg. It is then fractionated three times. 

The carcinogenic effects of these fractions are presented in figure 3 which clearly shows that almost the full activity remains in the small fraction containing 4-7 ring PAH, which is only 3.5% by weight of the total condensate Moreover, this fraction follows the same dose-response relation as the crude condensate (fig 4),... 

During operation, sour feed is mixed with hydrogen and heated in a fired furnace. The heated mixture is sent to a reactor where the hydrogen combines with the sulfur to form hydrogen sulfide. When the temperature is lowered slightly, the sweet crude condenses, leaving the hydrogen sulfide in a vapor state. This vapor-and-liquid mixture is sent to a separator where the low-sulfur sweet... 

Only the MgCl2 and CaCl2 salts in crude oil decompose to HCI at temperatures above 350 F. This HCI is very hydroscopic. That is, the first drop of water that condenses in the overhead condensers will absorb all the HCI it contacts. This leads to a very low localized pH. The operators see the effect of the hydroscopic nature of HCI as extremely accelerated localized corrosion at the inlets to the overhead crude condensers. 

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