Rectifying distillation

Semivolatile and non-volatile compounds of wood change the colour of the distillate and contribute to an up-rounded flavour. The wooden barrels which are permeable allow air to pass in and cause ethanol to evaporate thus, the ethanol content decreases and the aroma gets more intense, complex, and concentrated. Also harsher aroma constituents are removed and the spirit changes to mellow. The period of maturation depends on the size of the casks used, the alcoholic strength, as well as the temperature and humidity in the warehouse which leads to a smoother flavour. For production of neutral highly rectified distilled spirits like vodka, grain spirit, or white rum, the quality of water is of utmost importance to the flavour. In vodka production different treatments of water like de-... 

ALCOHOL OF WINE — (sometimes termed Distilled Wine) is thus called when every superfluity of wine has been so purged away that the whole is consumed and neither dregs nor moisture remain in the retort. The most subtle powder that can be made. If alcohol of wine be added, it is rectified, distilled wine. 

After approx. 48 h of fermentation, the fermented mash shows an alcohol content of approx. 6-10% by vol. When distilled in continuous stills with 3 or more colunms, the alcohol level in the distillate can be enriched up to 96.6% by vol. The purification of the raw distillate is normally carried out in continuous rectification equipment, for which the raw alcohol is usually diluted to approx. 15% by vol. before rectification in order to better separate fusel oil components. The first fractions of the rectified distillate - the so-called head fraction - contain significant quantities of acetaldehyde, methyl alcohol and low-boiling esters the middle part - heart fraction - represents so-called neutral spirits with an alcohol content of approx. 96.6% by vol. The tail fractions contain higher alcohols and higher esters etc. Since head and tail fractions contain organoleptic properties undesirable for neutral alcohol, they usually are employed as technical alcohol or have lately also been isolated and used as starting raw materials for the production of natural aroma components. 

Macerate for 1-2 days without adding water, distil slowly under vacuum. While the distillate is still running, add water and de-alcoholise to zero. Catch tails separately. Set in cool storage for 24 hours and filter. Rectify distillate to 72% v/v. 

Distillation.—Distillation is carried on in pot stills. The whole process must be carried out with a great deal of care. The first distillate has a nauseating odor and a raw burning taste so that it must be rectified to eliminate objectionable ethers, aldehydes and acids. It is also customary to trap off a portion of the total rectified distillate so that it may be used for blending with succeeding distillates. 

Direction for distillation same as preceding formula except that 20 gallons of rectified distillate at 60% are obtained. 

Highly rectified Distilled more then once. 

Although simple and countercurrent (rectified) distillation are among the most important physical separating methods employed in chemical industry, and hence also in research and works laboratories, it is often found that the apparatus used for this purpose in the laboratory has a low efficiency by present-day standards. Furthermore, calculations on the process are seldom made instead, the work is as a rule based entirely on experience and empirical data. 

Apparatus from standard parts for a) simple distillation, b) rectified distillation... 

Rectified distillation, with a column, may be carried out at pressures down to about 0.5 mm Hg. At lower pressures special forms of apparatus must be employed. 

The impurity of MeOH in the rectifier distillate a o2(meoh) was fixed at 1 mol% MeOH by varying the distillate flow rate D2. 

Introduce complex distillation configurations. Introduce prefractionation arrangements (with or without thermal coupling), side-rectifiers, and side-strippers to the extent that operability can be... 

Cinnamic acid can be readily esterified by the Fischer-Speier method without any risk of the addition of hydrogen chloride at the double bond. Proceed precisely as for the preparation of ethyl benzoate (p. 104), using 20 g. of cinnamic acid and 20 ml. of rectified spirit. When the crude product is poured into water, a sharp separation of the ester is not readily obtained, and hence the addition of about 10 ml. of carbon tetrachloride is particularly desirable. Finally distil off the carbon... 

Choice of solvent for recrystallisation. Obtain small samples (about 0 5 g.) of the following compounds from the storeroom (i) salicylic acid, (Li) acetanilide, (iii) m-dinitrobenzene, (iv) naphthalene, and (v) p-toluene-sulphonamide. Use the following solvents distilled water, methylated spirit, rectified spirit, acetone, benzene and glacial acetic acid. 

Place 50 g. of anhydrous calcium chloride and 260 g. (323 ml.) of rectified spirit (95 per cent, ethyl alcohol) in a 1-litre narrow neck bottle, and cool the mixture to 8° or below by immersion in ice water. Introduce slowly 125 g. (155 ml.) of freshly distilled acetaldehyde, b.p. 20-22° (Section 111,65) down the sides of the bottle so that it forms a layer on the alcoholic solution. Close the bottle with a tightly fitting cork and shake vigorously for 3-4 minutes a considerable rise in temperature occurs so that the stopper must be held well down to prevent the volatilisation of the acetaldehyde. Allow the stoppered bottle to stand for 24-30 hours with intermittent shaking. (After 1-2 hours the mixture separates into two layers.) Separate the upper layer ca. 320 g.) and wash it three times with 80 ml. portions of water. Dry for several hours over 6 g. of anhydrous potassium carbonate and fractionate with an efficient column (compare Section 11,17). Collect the fraction, b.p. 101-104°, as pure acetal. The yield is 200 g. 

Place 200 g, (250 ml.) of rectified spirit in a 1-litre round-bottomed flask fitted with a reflux condenser. Cool in ice and run in, slowly and with frequent shaking, 200 g. (109 ml.) of concentrated sulphuric acid. Add 83 g. (104 ml.) of -butyl cyanide (Section 111,113) to the mixture and reflux the whole for 10 hours. Allow to cool, pour the reaction mixture into ice water, separate the upper layer of ester and alcohol, and dry over anhydrous magnesium or calcium sulphate. Distil through a fractionating column and collect the ethyl n-valerate at 143-146°. A further amovmt of the pure ester may be obtained by redrying the fraction of low boiling point and redistilling. The yield is 110 g. 

Di lve 20 g. of the cyano ester in 100 ml. of rectified spirit and add a solution of 19 2 g. of pure potassium cyanide in 40 ml. of water. Allow to stand for 48 hours, then distil oflF the alcohol on a water bath. Add a large excess of concentrated hydrochloric acid and heat under reflux for 3 hours. Dilute with water, saturate the solution with ammonium sulphate, and extract with four 75 ml. portions of ether. Dry the combined ethereal extracts with anhydrous sodium or magnesium sulphate, and distil off the ether. RecrystaUise the residual acid from excess concentrated hydrochloric acid, and dry in the air. The yield of pure ew-dimethyl-succinic acid, m.p. 141-142°, is 12 g. 

Di-n-hexyl sulphide. Use 83 g. (71 ml.) of n-hexyl bromide (Section III.37), 56 g. of finely-powdered, anhydrous sodium sulphide and 100 ml. of rectified spirit. Reflux on a water bath for 20 hours. Distil ofiF the alcohol from a water bath very Uttle sulphide is obtained upon adding excess of water to the distiUate. Add excess of water to the residue in the flask and separate the upper layer of crude n-hexyl sulphide. Purify as for n-propyl sulphide, but distil under reduced pressure. CoUectthe n-hexyl sulphide at 113-114°/4 mm. The yield is 45 g. 

Equip a 500 ml. three-necked flask with an efficient stirrer (e.g., a Hershberg stirrer. Fig. II, 7, 8) and a reflux condenser stopper the third neck. Place a solution of 30 g. of sodium hydroxide in 100 ml. of water, and also 20-5 g. (17-1 ml.) of pure nitrobenzene in the flask, immerse it in a water bath maintained at 55-60°, and add 21 g. of anhydrous dextrose in small portions, with continuous stirring, during 1 hour. Then heat on a boiUng water bath for 2 hours. Pour the hot mixture into a 1 litre round-bottomed flask and steam distil (Fig. II, 40, 1) to remove aniline and nitrobenzene. When the distillate is clear (i.e., after about 1 htre has been collected), pour the residue into a beaker cooled in an ice bath. The azoxybenzene soon sohdifies. Filter with suction, grind the lumps of azoxybenzene in a mortar, wash with water, and dry upon filter paper or upon a porous plate. The yield of material, m.p. 35-35-5°, is 13 g. Recrystallise from 7 ml. of rectified spirit or of methyl alcohol the m.p. is raised to 36°. ... 

Equip a 1 Utre three-necked flask or a 1 litre bolt- head flask with a reflux condenser and a mercury-sealed stirrer. Dissolve 50-5 g. of commercial 2 4-dinitro-l-chlorobenzene in 250 ml. of rectified spirit in the flask, add the hydrazine solution, and reflux the mixture with stirring for an hour. Most of the condensation product separates during the first 10 minutes. Cool, filter with suction, and wash with 50 ml. of warm (60°) rectified spirit to remove unchanged dinitrochlorobenzene, and then with 50 ml. of hot water. The resulting 2 4-dinitrophenylhydrazine (30 g.) melts at 191-192° (decomp.), and is pure enough for most purposes. Distil oflF half the alcohol from the filtrate and thus obtain a less pure second crop (about 12 g.) recrystallise this from n-butyl alcohol (30 ml. per gram). If pure 2 4-dinitrophenylhydrazine is required, recrystallise the total yield from n-butyl alcohol or from dioxan (10 ml. per gram) this melts at 200° (decomp.). 

In a 1 litre round-bottomed flask provided with an efficient double surface condenser, place 40 g. (39 ml.) of aniline, 50 g. (40 ml.) of carbon sulphide CAUTION inflammable) (1), and 50 g. (63-5 ml.) of absolute ethyl alcohol (2). Set up the apparatus in the fume cupboard or attach an absorption device to the top of the condenser (see Fig. 11, 8, 1) to absorb the hydrogen sulphide which is evolved. Heat upon an electrically-heated water bath or upon a steam bath for 8 hours or until the contents of the flask sohdify. When the reaction is complete, arrange the condenser for downward distillation (Fig. 11, 13, 3), and remove the excess of carbon disulphide and alcohol (CA UTION inflammable there must be no flame near the receiver). Shake the residue in the flask with excess of dilute hydrochloric acid (1 10) to remove any aniline present, filter at the pump, wash with water, and drain well. Dry in the steam oven. The yield of crude product, which is quite satisfactory for the preparation of phenyl iao-thiocyanute (Section IV.95), is 40-45 g. Recrystalhse the crude thiocarbanihde by dissolving it, under reflux, in boiling rectified spirit (filter through a hot water funnel if the solution is not clear), and add hot water until the solution just becomes cloudy and allow to cool. Pure sj/m.-diphenylthiourea separates in colourless needles, m.p, 154°,... 

P-Hydroxy-a-naphthaldehyde, Equip a 1 litre three-necked flask with a separatory funnel, a mercury-sealed mechanical stirrer, and a long (double surface) reflux condenser. Place 50 g. of p-naphthol and 150 ml. of rectified spirit in the flask, start the stirrer, and rapidly add a solution of 100 g. of sodium hydroxide in 210 ml. of water. Heat the resulting solution to 70-80° on a water bath, and place 62 g. (42 ml.) of pure chloroform in the separatory funnel. Introduce the chloroform dropwise until reaction commences (indicated by the formation of a deep blue colour), remove the water bath, and continue the addition of the chloroform at such a rate that the mixture refluxes gently (about 1 5 hours). The sodium salt of the phenolic aldehyde separates near the end of the addition. Continue the stirring for a further 1 hour. Distil off the excess of chloroform and alcohol on a water bath use the apparatus shown in Fig. II, 41, 1, but retain the stirrer in the central aperture. Treat the residue, with stirring, dropwise with concentrated hydrochloric acid until... 

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