Apparatus columns

Mulopo, J.L., et al.. Experimental simulation of distillation column concentration profiles using a batch apparatus Columns stripping section. Chemical Engineering Science, 2005, 60(24) 6815 6823. 

Experiment 6. Fractional Distillation of a Mixture of Benzene and Toluene. Fractionally distil about 40 ml. of a mixture of equal volumes of benzene and toluene, using the type of fractionating column shown in Fig. ii(b), in which about 18-20 cm. of the column are actually filled with glass sections, but in which the cotton-wool lagging is not used. Distil very slowlyy so that the total distillation occupies about hours. Shield the apparatus very carefully from draughts. Collect the fractions having the b.ps (a) 80-85°, ( ) 85-107°, (c) 107-111°. A sharp separation should be obtained, e.g.y these fractions should have volumes of about 19, 2, and 17 ml. respectively. 

Use the apparatus detailed in Section 111,20. Dissolve 100 g. (123 ml.) of methyl n-butyl ketone (2-hexanone) (Section 111,152) in 750 ml. of ether and add 150 ml. of water. Introduce 69 g. of clean sodium in the form of wire (or small pieces) as rapidly as possible the reaction must be kept under control and, if necessary, the flask must be cooled in ice or in running water. When all the sodium has reacted, separate the ethereal layer, wash it with 25 ml. of dilute hydrochloric acid (1 1), then with water, dry with anhydrous potassium carbonate or with anhydrous calcium sulphate, and distil through a fractionating column. Collect the fraction of b.p. 136-138°. The yield of methyl n-butyl carbinol (2-hexanol) is 97 g. 

Reflux a mixture of 68 g. of anhydrous zinc chloride (e.g., sticks), 40 ml. (47 -5 g.) of concentrated hydrochloric acid and 18-5 g. (23 ml.) of sec.-butyl alcohol (b.p. 99-100°) in the apparatus of Fig. 777, 25, 1 for 2 hours. Distil oflF the crude chloride untU the temperature rises to 100°. Separate the upper layer of the distillate, wash it successively with water, 5 per cent, sodium hydroxide solution and water dry with anhydrous calcium chloride. Distil through a short column or from a Claisen flask with fractionating side arm, and collect the fraction of b.p. 67-70° some high boiling point material remains in the flask. Redistil and collect the pure cc. butyl chloride at 67-69°. The yield is 15 g. 

Fit up the apparatus shown in Fig. Ill, 61, 1. The bolt-head flask is of 500 ml. capacity and the Hempel column is fllled with glass rings... 

Alternatively—and this procedure is recommended—remove the ether with the apparatus shown in Fig. II, 13, 4. A slightly improved yield is obtained if a short fractionating column is used. 

Apparatus 1-1 flask (see Fig. 1) for the addition of bromine 1-1 two-necked flask, provided with a dropping funnel and a 40-cm Vigreux column, for the dehydrohalo-genation the Vigreux column was connected to a condenser and receiver, cooled at -75°C. 

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