Distillation column overhead separator

C The feed to a distillation column is separated into net overhead product containing nothing... 

Knockout pot (drums and accumulators for high ratios of liquid/gas, as in distillation column overheads) use horizontal cylinder size vapor space to provide the residence time for drops to settle out. Vapor volume between 20 and 50% with a minimum of 0.3 m. Design vapor-phase cross-sectional area to allow drops to settle in assigned length of the drum. Assume drops 0.1 to 2(X) pm. The Souders-Brown separation maximum superficial gas velocity is... 

Example 12-1 Design a continuous fractionating distillation column to separate 3.78 kg/sec of 40 percent benzene and 60 percent toluene into an overhead product containing 97 mass percent benzene and a bottom product containing 98 mass percent toluene. Use a reflux ratio of 3.5 mole to 1 mole of product. Latent molal heat of both benzene and toluene is about 357.1 kJ/kg. 

In the first class, azeotropic distillation, the extraneous mass-separating agent is relatively volatile and is known as an entrainer. This entrainer forms either a low-boiling binary azeotrope with one of the keys or, more often, a ternary azeotrope containing both keys. The latter kind of operation is feasible only if condensation of the overhead vapor results in two liquid phases, one of which contains the bulk of one of the key components and the other contains the bulk of the entrainer. A t3q)ical scheme is shown in Fig. 3.10. The mixture (A -I- B) is fed to the column, and relatively pure A is taken from the column bottoms. A ternary azeotrope distilled overhead is condensed and separated into two liquid layers in the decanter. One layer contains a mixture of A -I- entrainer which is returned as reflux. The other layer contains relatively pure B. If the B layer contains a significant amount of entrainer, then this layer may need to be fed to an additional column to separate and recycle the entrainer and produce pure B. 

In France, Compagnie Europnene du Zirconium (CEZUS) now owned jointly by Pechiney, Eramatome, and Cogema, uses a separation (14) based on the extractive distillation of zirconium—hafnium tetrachlorides in a molten potassium chloride—aluminum trichloride solvent at atmospheric pressure at 350°C. Eor feed, the impure zirconium—hafnium tetrachlorides from the zircon chlorination are first purified by sublimation. The purified tetrachlorides are again sublimed to vapor feed the distillation column containing the solvent salt. Hafnium tetrachloride is recovered in an enriched overhead fraction which is accumulated and reprocessed to pure hafnium tetrachloride. 

The methyl ethyl ketazine forms an immiscible upper organic layer easily removed by decantation. The lower, aqueous phase, containing acetamide and sodium phosphate, is concentrated to remove water formed in the reaction and is then recycled to the reactor after a purge of water-soluble impurities. Organic by-products are separated from the ketazine layer by distillation. The purified ketazine is then hydrolyzed under pressure (0.2—1.5 MPa (2—15 atm)) to give aqueous hydrazine and methyl ethyl ketone overhead, which is recycled (122). The aqueous hydrazine is concentrated in a final distillation column. 

The oxidation reactor effluent and methanol ate sent to the esterification reactor, which operates at up to 250°C and a pressure sufficient to maintain the Hquid phase. This latter is about 2500 kPa (25 atm). The oxidation products are converted to methyl -toluate and dimethyl terephthalate without a catalyst. Excess methanol is suppHed, and steam and vaporized methanol ate removed and enter a methanol recovery column. The esterification products flow to a cmde ester column, which separates the toluate from the terephthalate. The overhead stream of methyl -toluate is returned to the oxidation reactor, and the bottoms stream of dimethyl terephthalate goes to a primary distillation. The distillate is dissolved in methanol, crystallized, and sohd dimethyl terephthalate is recovered. The dimethyl terephthalate can then be either recrystallized or distilled to yield the highly pure material needed for the polyesterification reaction. 

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. 

Figure 5 illustrates a typical distillation train in a styrene plant. Benzene and toluene by-products are recovered in the overhead of the benzene—toluene column. The bottoms from the benzene—toluene column are distilled in the ethylbenzene recycle column, where the separation of ethylbenzene and styrene is effected. The ethylbenzene, containing up to 3% styrene, is taken overhead and recycled to the dehydrogenation section. The bottoms, which contain styrene, by-products heavier than styrene, polymers, inhibitor, and up to 1000 ppm ethylbenzene, are pumped to the styrene finishing column. The overhead product from this column is purified styrene. The bottoms are further processed in a residue-finishing system to recover additional styrene from the residue, which consists of heavy by-products, polymers, and inhibitor. The residue is used as fuel. The residue-finishing system can be a flash evaporator or a small distillation column. This distillation sequence is used in the Fina-Badger process and the Dow process. 

Medium Boiling Esters. Esterificatioa of ethyl and propyl alcohols, ethylene glycol, and glycerol with various acids, eg, chloro- or bromoacetic, or pymvic, by the use of a third component such as bensene, toluene, hexane, cyclohexane, or carbon tetrachloride to remove the water produced is quite common. Bensene has been used as a co-solvent ia the preparatioa of methyl pymvate from pymvic acid (101). The preparatioa of ethyl lactate is described as an example of the general procedure (102). A mixture of 1 mol 80% lactic acid and 2.3 mol 95% ethyl alcohol is added to a volume of benzene equal to half that of the alcohol (ca 43 mL), and the resulting mixture is refluxed for several hours. When distilled, the overhead condensate separates iato layers. The lower layer is extracted to recover the benzene and alcohol, and the water is discarded. The upper layer is returned to the column for reflux. After all the water is removed from the reaction mixture, the excess of alcohol and benzene is removed by distillation, and the ester is fractionated to isolate the pure ester. 

In the use of temperature measurement for control of the separation in a distillation column, repeatability is crucial but accuracy is not. Composition control for the overhead product would be based on a measurement of the temperature on one of the trays in the rectifying section. A target would be provided for this temperature. However, at periodic intervals, a sample of the overhead product is analyzed in the laboratory and the information provided to the process operator. Should this analysis be outside acceptable limits, the operator would adjust the set point for the temperature. This procedure effectively compensates for an inaccurate temperature measurement however, the success of this approach requires good repeatability from the temperature measurement. 

The crude liquid chlorobenzenes stream leaving the second reactor is washed with water and caustic soda solution to remove all dissolved hydrogen chloride. The product recovery system consists of two distillation columns in series. In the first column (the benzene column ) unreacted benzene is recovered as top product and recycled. In the second column (the chlorobenzene column ) the mono- and dichlorobenzenes are separated. The recovered benzene from the first column is mixed with the raw benzene feed and this combined stream is fed to a distillation column (the drying column ) where water is removed as overhead. The benzene stream from the bottom of the drying column is fed to the reaction system. 

The bottom product from column (G) passes to the hydroextractive distillation column (H). The water feed rate to column (H) is five times that of the bottom product flow from column (G). It may be assumed that the acetonitrile and other by-products are discharged as bottom product from column (H) and discarded. The overhead product from column (H), consisting of the acrylonitrile water azeotrope, is condensed and passed to a separator. The lower aqueous layer is returned to column (H). 

Example 9.1 A distillation column operating at 14 bar with a saturated liquid feed of 1000 kmoUr1 with composition given in Table 9.1 is to be separated into an overhead product that recovers 99% of the n-butane overhead and 95% of the i-pentane in the bottoms. Relative volatilities are also given in Table 9.1. 

In this approach accident cases and design recommendations can be analysed level by level. In the database the knowledge of known processes is divided into categories of process, subprocess, system, subsystem, equipment and detail (Fig. 6). Process is an independent processing unit (e.g. hydrogenation unit). Subprocess is an independent part of a process such as reactor or separation section. System is an independent part of a subprocess such as a distillation column with its all auxiliary systems. Subsystem is a functional part of a system such as a reactor heat recovery system or a column overhead system including their control systems. Equipment is an unit operation or an unit process such as a heat exchanger, a reactor or a distillation column. Detail is an item in a pipe or a piece of equipment (e.g. a tray in a column, a control valve in a pipe). 

Process designers sometimes like to use dephlegmators or partial condensers mounted directly in the top of the distillation column when the overhead product is taken off as a vapor. They arc particularly popular for corrosive, toxic, or hard-to-handle chemicals since they eliminate a. separate condenser shell, a reflux drum, and a reflux pump. Comment on the relative controllability of the two process systems sketched below. 

The reactor effluent is separated in a distillation column. The overhead is mostly excess reactant A which is recycled back to the reactor. The bottoms from the column is mostly product C. The reaction occurs in the liquid phase so the reactor feed streams are liquid. Reactant B is added directly to the reactor on flow control. The flow rate of the recycle stream is ratioed to the flow rate of the B feed stream. The composition of A in the column base sets heat input. The composition of C in the column overhead sets reflux. 

The overhead stream of the distillation column may be a low-boiling binary azeotrope of one of the keys with the entrainer or more often a ternary azeotrope containing both keys. The latter kind of operation is feasible only if condensation results in two liquid phases, one of which contains the bulk of one of the key components and the other contains virtually all of the entrainer which can be returned to the column. Figure 13.29(a) is of such a flow scheme. When the separation resulting from the phase split is... 

Benzene and toluene by-products are recovered in the overhead of the benzene-toluene distillation column. The bottoms from the benzene-toluene column are distilled in the ethylbenzene recycle column, where the separation of ethylbenzene and styrene is effected. The bottoms, are pumped to file styrene finishing column. The overhead product from this column is purified styrene. The bottoms are further processed in a residue-finishing system to recover additional styrene from the residue. 

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