Distillation alcohol

Alternatively, the following procedure for isolating the glycol may be used. Dilute the partly cooled mixture with 250 ml. of water, transfer to a distilling flask, and distil from an oil bath until the temperature reaches 95°. Transfer the hot residue to an apparatus for continuous extraction with ether (e.g.. Fig. II, 44, 2). The extraction is a slow process (36-48 hours) as the glycol is not very soluble in ether. (Benzene may also be employed as the extraction solvent.) Distil off the ether and, after removal of the water and alcohol, distil the glycol under reduced pressure from a Claisen flask. 

If the original ester is a fat or oil and produces an odour of acrolein when heated, it may be a glyceride. Esters of ethylene glycol and of glycol with simple fatty acids are viscous and of high b.p. They are hydrolysed (method I) and the ethyl alcohol distilled ofl. The residue is diluted (a soap may be formed) and acidified with hydrochloric acid (Congo red paper). The acid is filtered or... 

Treat the combined distiUates of b.p. 195-260° with anhydrous potassium carbonate to neutralise the Uttle formic acid present and to salt out the allyl alcohol. Distil the latter through a fractionating column and collect the fraction of b.p, up to 99° separately this weighs 210 g, and consists of 70 per cent, allyl alcohol. To obtain anli5 dious allyl alcohol, use either of the following procedures —... 

Preparation of benzyl cyanide. Place 100 g. of powdered, technical sodium cyanide (97-98 per cent. NaCN) (CAUTION) and 90 ml. of water in a 1 litre round-bottomed flask provided with a reflux condenser. Warm on a water bath until the sodium cyanide dissolves. Add, by means of a separatory funnel fitted into the top of the condenser with a grooved cork, a solution of 200 g. (181-5 ml.) of benzyl chloride (Section IV.22) in 200 g. of rectified spirit during 30-45 minutes. Heat the mixture in a water bath for 4 hours, cool, and filter off the precipitated sodium chloride with suction wash with a little alcohol. Distil off as much as possible of the alcohol on a water bath (wrap the flask in a cloth) (Fig. II, 13, 3). Cool the residual liquid, filter if necessary, and separate the layer of crude benzyl cyanide. (Sometimes it is advantageous to extract the nitrile with ether or benzene.) Dry over a little anhydrous magnesium sulphate, and distil under diminished pressure from a Claisen flask, preferably with a fractionating side arm (Figs. II, 24, 2-5). Collect the benzyl cyanide at 102-103°/10 mm. The yield is 160 g. 

Diethylene glycol method. Place 0-5 g. of potassium hydroxide pellets, 3 ml. of diethylene glycol and 0 5 ml. of water in a 10 or 25 ml. distilling flask heat the mixture gently until the alkali has dissolved and cool. Add 1-2 g. of the ester and mix well. Fit the flask with a thermometer and a small water-cooled condenser in the usual way. Heat the flask over a small flame whilst shaking gently to mix the contents. When only one liquid phase, or one hquid phase and one solid phase, remains in the flask, heat the mixture more strongly so that the alcohol distils. Identify the alcohol in the distillate by the preparation of the 3 5 dinitrobenzoate (Section 111,27,2). 

Alcohol distillation Alcohol fractionation Alcohol free beer... 

The aqueous layer from the ester column distillate, the raffinate from washing the ester, and the aqueous phase from the dehydration step are combined and distilled in the alcohol stripper. The wet alcohol distillate containing a low level of acrylate is recycled to the esterification reactor. The aqueous column bottoms are incinerated or sent to biological treatment. Biological treatment is common. 

Evaporation and Distillation. Steam is used to supply heat to most evaporation (qv) and distillation (qv) processes, such as ia sugar-juice processiag and alcohol distillation. In evaporation, pure solvent is removed and a low volatiUty solute is concentrated. Distillation transfers lower boiling components from the Hquid to the vapor phase. The vapors are then condensed to recover the desired components. In steam distillation, the steam is admitted iato direct coatact with the solutioa to be evaporated and the flow of steam to the condenser is used to transport distillates of low volatiHty. In evaporation of concentrated solutions, there may be substantial boiling poiat elevation. For example, the boiling poiat of an 80% NaOH solution at atmospheric pressure is 226°C. 

Alcohols Moderate- to high-molecular-weight monohydric and polyhydric alcohols octyl alcohol C-12 to C-20 alcohols laiiryl alcohol Distillation fermentation papermaking glues and adhesives... 

The term still is applied only to the vessel in which liquids are boiled during distillation, but the term is sometimes applied to the entire apparatus, including the fractionating column, the condenser, and the receiver in which the distillate is collected. If a water and alcohol distillate is returned from the condenser and made to drip down through a long column onto a series of plates, and if the vapor, as it rises to the condenser, is made to bubble through this liquid at each plate, the vapor and liquid will interact so that some of the water in the vapor condenses and some of the alcohol in the liquid vaporizes. The interaction at each plate is equivalent to a redistillation. This process is referred to by several names in the industry namely rectification, fractionation, or fractional distillation. 

In a dry, 250 ml, three-necked flask equipped with a dropping funnel and magnetic stirrer are placed 40 ml of dry /-butyl alcohol (distilled from calcium hydride) and 4.0 g (0.036 mole) of potassium /-butoxide. The solution is cooled in ice and 40 g (49 ml, 0.49 mole) of dry cyclohexene is added. Bromoform (10 g, 3.5 ml, 0.039 mole) is added to the cooled, stirred reaction vessel dropwise over about hour, and the vessel is stirred an additional hour with the ice bath removed. The reaction mixture is poured into water (approx. 150 ml), and the layers are separated. The aqueous layer is extracted with 25 mi of pentane, and the extract is combined with the organic layer. The combined layers are dried (sodium sulfate), and the solvent is removed. The product is purified by distillation, bp 10078 mm. 

Ethyl 4-i-butylphenylmalonate (27.53 g) in absolute alcohol (25 ml) was added with stirring to a solution of sodium ethoxide from sodium (2.17 g) in absolute alcohol (75 ml). Ethyl iodide (15 ml) was added and the mixture refluxed for 2 A hours, the alcohol distilled and the residue diluted with water, extracted with ether, washed with sodium bisulfite, water, and evaporated to dryness. 

The apparatus consists of a 3-]. three-necked flask fitted with a mercury-sealed mechanical stirrer, a reflux condenser, a dropping funnel, and a thermometer which reaches almost to the bottom of the flask. Five hundred grams of potassium hydroxide pellets (85 per cent potassium hydroxide) (7.5 moles) and 750 cc. of commercial absolute methyl alcohol (free from acetone) are placed in the flask and stirring begun. The bulk of the alkali dissolves in a few minutes, with the evolution of heat. The flask is now surrounded by an ample cold-water bath, and, when the internal temperature drops to 6o°, addition of a mixture of 360 g. (353 cc., 3 moles) of -tolualdehyde (Note 1), 300 cc. of formalin (3.9 moles) (Note 2), and 300 cc. of absolute methyl alcohol is begun at such a rate that the internal temperature remains at 60-70°. This addition requires about fifteen minutes. The internal temperature is then maintained at 60-70° for three hours, after which the reflux condenser is replaced by a downward condenser, and the methyl alcohol distilled with the aid of a brine bath until the internal temperature reaches ioi°. Nine hundred cubic centimeters of cold water is then added to the warm residue, and the mixture cooled. The resulting two layers are separated at once (Note 3), and the aqueous layer extracted with three 200-cc. portions of benzene. The combined oil and extracts are washed with five or six 50-cc. portions of water (Note 4), and the combined washings extracted... 

Durene is quite volatile, and should not be allowed to remain exposed to the air any longer than necessary. It is also quite volatile with alcohol, and the mother liquors resulting from the recrystallizations should be distilled the alcoholic distillate is used for further recrystallizations, and the residues may be worked up for durene by heating with aluminium chloride. 

The contents of the flask are transferred to a separatory funnel while still hot and washed three times with 200-cc. portions of hot water to remove the sodium laurate (Note 7). The lauryl alcohol is extracted with ether from the cooled mixture and the washings. The combined ether extracts are washed with water, sodium carbonate solution, and again with water, and dried over anhydrous magnesium sulfate. The ether is evaporated and the lauryl alcohol distilled under diminished pressure. The yield is 60-70 g. (65-75 per cent of the theoretical amount) of a product boiling at i43-i46°/i8 mm. or i98-2oo°/i35 mm. (Note 8). 

By diluting the alcoholic distillate from the reaction mixture with io 1. of water, it is possible to recover about 400 g. of ethylene dibromide. 

A mixture of 105.7 g. (0.55 mole) of ethyl benzoylacetate and 46.6 g. (0.5 mole) of aniline (Note 1) is placed in the dropping funnel D (Fig. 1) at the top of the continuous reactor (Notes 2 and 3) after the column has been heated to 135° (transformer set at 80 volts) (Notes 4 and 5). The reactants are then admitted to the column during about 15 minutes (this corresponds to a rate of amide formation of 396-400 g. per hour). Alcohol distils (Note 5) noticeably from the column during the addition and collects in flask G. At the completion of the reaction,... 

In the aqueous-alcoholic distillate having a volume of about 200 c.c. about 70 c.c. or 56 g. of alcohol will be found. The yield of alcohol approaches the theoretical value and should amount to about 20 per cent more than would be calculated from the maltose determination just carried out, since the latter does not, of course, take into account the additional sugar produced during the fermentation by diastatic after effect . 

In order to obtain the alcohol in the pure state the final distillate is dropped from a tap funnel into a distilling flask containing 700 g. of quicklime. The flask is connected to a downward condenser and is heated in an oil bath so that the alcohol distils. 

Reagent grade i-butyl alcohol distilled from calcium hydride was used. 

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