Extractive distillation Volume

When butadiene is produced in olefins plants or in refinery crackers, they come mixed with relatively large volumes of the other C4 family. Sometimes the other C4S need not be separated from each other, for example if they are going to be used for allcylation plant feed. In that case, the butadiene can be separated from the other C4S by extractive distillation. This process uses a solvent that will preferentially dissolve butadiene, ignoring the other components in the stream. 

The topic covered in the 10 papers of the first section is commonly referred to as salt effect in vapor-liquid equilibrium and is potentially of great industrial importance. This salt effect leads to extractive distillation processes in which a dissolved salt replaces a liquid additive as the separating agent the replacement often results in a greatly improved separating ability and reduced energy requirements. Two papers in this volume, those by Sloan and by Vaillancourt, illustrate the use of such processing to concentrate nitric acid from its aqueous azeotrope. Nevertheless, the effect has not been exploited by industry to nearly the extent that would seem to be merited by its scientific promise. 

If the extract E calculated indirectly lies between 3 and 4, such volume of the wine is measured out from a burette as will give not more than 1 5 gram of extract, distilled water being then added to bring the volume up to 50 c.c. The volume of wine to be taken is found by dividing 150 by the value of E found in the table. The diluted wine is evaporated in a tared dish as described above and the extract per litre of the wine calculated. 

Data of Azeotropes. The choice of an azeotropic entrainer for a desired separation is much more restricted than that of solvents for extractive distillation, although many azeotropic data are known. The most modern and extensive compilation is that of Gmehling et al. (1994), a two-volume set that includes many ternary and some quaternary azeotropes. Probably the most available... 

This case study involves the recovery of highly valued and high demand ethylbenzene (EB) and mixed-xylenes (comprising of p-xylene (PX), m-xylene (MX) and o-xylene (OX)) from a C8-aromatics mixture (C8A). As point out above, C8A is isomers mixture, so their separation (recovery) is not simple, that why there is only one commercial process of liquid-phase adsorptive separation available for EB recovery from C8A. [8] However, this process requires high investment cost and generates huge volume of waste adsorbent that may become an environmental problem. Therefore, another green process should be considered for the EB purification. The ratio of various properties of the key components (EB and PX) were tested to examine the possibly alternatives. The result showed, by vapor pressure ratio, the solvent-based extractive distillation can be employed for their purification. [7]... 

Eor extractive distillation, the solvent should have a boiling temperature 50 to 100°C higher than those of the products, with solubility parameters and molar volumes similar to those of one product but different from the other. 

When a decrease of the original volume (via solvent extraction, distillation, or evaporation, etc.) is required before analysis, back calculations must be carried out to determine the original volume that must be collected to give the desired measurable level of the parameter. For example, if Vj is the volume calculated from the use of Ms and R, then the required original volume Vq is obtained from the product of Vi and the volume reduction factor For a volume reduction of 100, Vo would be lOOVi. 

The interest in w-butanol as a biofuel has increased in recent years owing to its superior fuel qualities compared to ethanol. These include a higher octane number, lower heat of vaporization, higher energy density (energy/volume), and lower vapor pressure. However, in the traditional ABE (acetone-butanol-ethanol) fermentation process, the concentration of n-butanol coming from the fermenter is lower than that achieved in ethanol fermentation. In addition, acetone and ethanol are also produced. Recent studies to improve yield and increase w-butanol concentration have explored fed-batch systems with stripping, adsorption, liquid-liquid extraction, distillation, and/or pervaporation to recover products. 

In view of the small volume of nitromethane to be manipulated, the crude nitromethane may be extracted from the aqueous distillate with ether (30-40 ml.). Dry the ethereal extract over sodium sulphate, filter through a fluted filter-paper, and then distil off the ether on a water-bath with the usual precautions (Fig. 64, p. 163 Fig, 23(E), p. 45) finally distil the residual nitromethane. 

Place the distillate in a separating-funnel and extract the benzonitrile twice, using about 30 ml. of ether for each extraction. Return the united ethereal extracts to the funnel and shake with 10% sodium hydroxide solution to eliminate traces of phenol formed by decomposition of the benzenediazonium chloride. Then run off the lower aqueous layer, and shake the ethereal solution with about an equal volume of dilute sulphuric acid to remove traces of foul-smelling phenyl isocyanide (CaHjNC) which are always present. Finally separate the sulphuric acid as completely as possible, and shake the ether with water to ensure absence of acid. Run off the water and dry the benzonitrile solution over granular calcium chloride for about 20 minutes. 

Filter the dried extract, and then distil off the ether from a small flask, using the customary precautions if the volume of ether is large, fit a dropping-funnel to the flask so that the ethereal extract can be run into the flask as the ether distils off cf. Fig. 23(E), p. 45). When the ether has been removed, replace the water-condenser by an air-condenser, and continue... 

If no solid precipitate is obtained but the solution becomes cloudy, a low-melting or liquid phenol is indicated this will, of course, be revealed also by the characteristic phenolic odour. Transfer to a separating-funnel and extract with an equal volume of ether. Separate and dry with anhydrous sodium sulphate. Distil off the ether and identify the residue. 

If no solid precipitate is obtained, an oil or an oily suspension, may be produced. Allow to stand, and then, if possible, separate the oil directly in a separating Tunnel and dry with solid KOH. If the volume of the oil is too small for such separation, extract with ether and then separate the ethereal solution, dry as before, filter, and distil off the ether. Distil the amine (if considered necessary) and identify. 

Mix 50 ml. of formalin, containing about 37 per cent, of formaldehyde, with 40 ml. of concentrated ammonia solution (sp. gr. 0- 88) in a 200 ml. round-bottomed flask. Insert a two-holed cork or rubber stopper carrying a capillary tube drawn out at the lower end (as for vacuum distillation) and reaching almost to the bottom of the flask, and also a short outlet tube connected through a filter flask to a water pump. Evaporate the contents of the flask as far as possible on a water bath under reduced pressure. Add a further 40 ml. of concentrated ammonia solution and repeat the evaporation. Attach a reflux condenser to the flask, add sufficient absolute ethyl alcohol (about 100 ml.) in small portions to dissolve most of the residue, heat under reflux for a few minutes and filter the hot alcoholic extract, preferably through a hot water fuimel (all flames in the vicinity must be extinguished). When cold, filter the hexamine, wash it with a little absolute alcohol, and dry in the air. The yield is 10 g. Treat the filtrate with an equal volume of dry ether and cool in ice. A fiulher 2 g. of hexamine is obtained. 

IsoValeric acid. Prepare dilute sulphuric acid by adding 140 ml. of concentrated sulphuric acid cautiously and with stirring to 85 ml. of water cool and add 80 g. (99 ml.) of redistilled woamyl alcohol. Place a solution of 200 g. of crystallised sodium dicliromate in 400 ml. of water in a 1-litre (or 1-5 litre) round-bottomed flask and attach an efficient reflux condenser. Add the sulphuric acid solution of the isoamyl alcohol in amaU portions through the top of the condenser shake the apparatus vigorously after each addition. No heating is required as the heat of the reaction will suffice to keep the mixture hot. It is important to shake the flask well immediately after each addition and not to add a further portion of alcohol until the previous one has reacted if the reaction should become violent, immerse the flask momentarily in ice water. The addition occupies 2-2-5 hours. When all the isoamyl alcohol has been introduced, reflux the mixture gently for 30 minutes, and then allow to cool. Arrange the flask for distillation (compare Fig. II, 13, 3, but with the thermometer omitted) and collect about 350 ml. of distillate. The latter consists of a mixture of water, isovaleric acid and isoamyl isovalerate. Add 30 g. of potassium not sodium) hydroxide pellets to the distillate and shake until dissolved. Transfer to a separatory funnel and remove the upper layer of ester (16 g.). Treat the aqueous layer contained in a beaker with 30 ml. of dilute sulphuric acid (1 1 by volume) and extract the liberated isovaleric acid with two... 

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