Distillate yields

Maier, C.E., P.-H. Bigeard, A. Billon and P. Dufresne (1988), Boost middle distillate yield and quality with a new generation of hydrocracking catalyst . NPRA paper No. AM-88-76, Annual meeting, San Antonio, TX. 

Ethyl p-phenylethyl ketone. Use 100 g. of pure hydrocinnamic acid and 200 g. (201 -5 ml.) of pure propionic acid. Fractionation of the distillate yields 70 g. of diethyl ketone (b.p. 100-102°), 72 g. of ethyl p-phenyl-ethyl ketone (b.p. 245-249° the pure ketone boils at 248°), and 18 g, of crude di-p-phenylethyl ketone (high b.p. residue). 

This process yields a purely straight-chain acid of even carbon number. Typically, the value of n varies from two to six, and distillation yields the pure components. Du Pont pioneered the development of this technology. Allied has used hexafluoroacetone to produce telomer iodides containing the... 

Direct hydrohquefaction of biomass or wastes can be achieved by direct hydrogenation of wood chips on treatment at 10,132 kPa and 340 to 350°C with water and Raney nickel catalyst (45). The wood is completely converted to an oily Hquid, methane, and other hydrocarbon gases. Batch reaction times of 4 hours give oil yields of about 35 wt % of the feed the oil contains about 12 wt % oxygen and has a heating value of about 37.2 MJ /kg (16,000 Btu/lb). Distillation yields a significant fraction that boils in the same range as diesel fuel and is completely miscible with it. 

Gumylphenol. -Cumylphenol (PGP) or 4-(1-methyl-l-phenylethyl)phenol is produced by the alkylation of phenol with a-methylstyrene under acid catalysis. a-Methylstyrene is a by-product from the production of phenol via the cumene oxidation process. The principal by-products from the production of 4-cumylphenol result from the dimerization and intramolecular alkylation of a-methylstyrene to yield substituted indanes. 4-Cumylphenol [599-64-4] is purified by either fractional distillation or crystallization from a suitable solvent. Purification by crystallization results in the easy separation of the substituted indanes from the product and yields a soHd material which is packaged in plastic or paper bags (20 kg net weight). Purification of 4-cumylphenol by fractional distillation yields a product which is almost totally free of any dicumylphenol. The molten product resulting from purification by distillation can be flaked to yield a soHd form however, the soHd form of 4-cumylphenol sinters severely over time. PGP is best stored and transported as a molten material. 

After flashing the propylene, the aqueous solution from the separator is sent to the purification section where the catalyst is separated by a2eotropic distillation 88 wt % isopropyl alcohol is obtained overhead. The bottoms containing aqueous catalyst solution are recycled to the reactor, and the light ends are stripped of low boiling impurities, eg, diisopropyl ether and acetone. A2eotropic distillation yields dry isopropyl alcohol, and the final distillation column yields a product of more than 99.99% purity. 

From the produc t specifications, distillate yields are computed as follows From Fig. 13-86 and the ASTM D 86 50 percent temperatures, TBP 50 percent temperatures of the three intermediate cuts are obtained as 155, 236, and 316°C (311, 456, and 600°F) for the HN, LD, and HD respectively. The TBP cut points, corresponding volume fractions of crude oil, and flow rates of the four distillates are readily obtained by stai-ting from the specified 343°C (650°F) cut point as follows, where CP is tne cut point and T is the TBP temperature (°F) ... 

The submitter reports that operation of this procedure on a scale of 72 moles of paraformaldehyde gave a crude yield of 3601 g. (87%) and a distilled yield of 3519 g. (85%). 

Syntheses of Nicotine. Pictet and Cr pieux found that 3-aminopyridine mueate on dry distillation yielded l-(3-pyridyl)pyrrole (I), and this, in accordance with the usual behaviour of such pyrrole derivatives, transfers its pyridyl substituent from the 1- to the 2-position at a red heat giving 2-(3-pyridyl)pyrrole (II), which is nomieotyrine. The potassium derivative of this reacts with methyl iodide to form l-methjd-2-(3-pyridyl)-pyrrole methiodide, which is identical with nieotyrine methiodide (III), and on distillation with lime yields nieotyrine (IV Cl — CH). For a re-investigation of this synthesis see Spath and Kainrath. ... 

Hexane-2,5-dione (342 mg, 3 mmol) was thoroughly mixed with alumina (1 g) before HMDS (1 mL, 4.8 mmol) was added, and the mixture was heated at 100-110 °C until the hexamethyldisiloxane formed was completely evaporated (about 20 min). Once the mixture cooled down to rt, the product was eluted with CH2CI2 and the oil obtained after evaporation of the solvent was purified by distillation yield 231 mg (81%), bp 68 °C/18 Torn... 

The side-chain cyanoethylation of alkyl thienyl ketones with acrylonitrile has been studied " and used for the preparation of 8-oxonitriles and S-oxoacids. Aminomethylation (Mannich reaction) of 2-acetylthiophene followed by steam distillation yielded 50% of 2-thienyl vinyl ketone, and has also been used for the synthesis of compounds of biological interest. ... 

The alkylborane is then oxidized by the addition of 150 ml of a 15% solution of hydrogen peroxide, while the pH of the reaction mixture is maintained at 7-8 by the simultaneous addition of 3 Asodium hydroxide, the process being carried out at ice-bath temperature. The reaction mixture is neutralized and subjected to steam distillation. The distillate is extracted with ether, and the extract is dried over anhydrous magnesium sulfate. After removal of the ether, distillation yields 18.0 g (70%) of n-octanal, bp 83-85733 mm. 

Collected and dried ether extracts were evaporated and the residue vacuum distilled yielded 15 g of a thick oil of boiling point at 0.1 to 0.2 mm Hg 127t to 135°C. 

A) Preparation of p-Hydroxy-p -Methoxybemhydrylidenecyclohexane To a Grignard solution prepared from 110 g of magnesium (4.5 mols) and 840 g of p-bromoanisole (4.5 mols) in one liter of anhydrous ether, there was added dropwise with vigorous agitation 307 g of p-hydroxyphenyl cyclohexyl ketone (1.5 mols) dissolved in one liter of anhydrous ether. Upon completion of the addition the reaction mixture was refluxed for 2.5 hours with agitation, and was then cooled. Thereupon 15 mols of ammonium chloride dissolved in 3 liters of water were added. The ethereal layer was separated, washed with water, dried over anhydrous sodium sulfate and distilled. Yield 370 g. BP 180° to 190°C at 0.1 mm. The substance was recrystallized from a mixture of carbon tetrachloride and petroleum ether. MP 145° to 146°C. 

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