Rectifying section distillation

The rectifying section contains three or four bubble cap (wine) plates in the top section of the stiU to produce distillates up to 160° proof. Whiskey stills are usually made of copper, especially in the rectifying section, which often yields a superior product. Additional copper surface in the upper section of the column may be provided by a demister, a flat disk of copper mesh. Stainless steel is also used in some stills. 

Distillers employ a somewhat unique process to make various products and have tailored approaches to control and reduce ethyl carbamate to their own particular process. Some of the methods used are the use of copper packing in the rectifying section of stills, increased frequency of cleaning stills and other equipment, and using a cool-down period in the cleaning procedure. Increased rectification also reduces ethyl carbamate. Keeping the system clean is critical to minimising ethyl carbamate. 

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. 

In another alternative, shown in Fig. 13-3 7, the rectifying section may be operated at a pressure sufficiently higher than that of the stripping section such that heat can be transferred between any desired pairs of stages of the two sections. This technique, described by Mah et al. (op. cit.) and referred to as SRV (secondary reflux and vaporization) distillation, can result in a significant reduction in utihty requirements for the overhead condenser and bottoms reboiler. 

In the rectifying section, the equilibrium relationship for component at any stage n can be expressed in terms of component flow rate in the distillate d = Dxd and component absorption factor A = hjKiS... 

The rate-based model gave a distillate with 0.023 mol % ethylbenzene and 0.0003 mol % styrene, and a bottoms product with essentially no methanol and 0.008 mol % toluene. Miirphree tray efficiencies for toluene, styrene, and ethylbenzene varied somewhat from tray to tray, but were confined mainly between 86 and 93 percent. Methanol tray efficiencies varied widely, mainly from 19 to 105 percent, with high values in the rectifying section and low values in the stripping section. Temperature differences between vapor and liquid phases leaving a tray were not larger than 5 F. 

Figure 9.6 Mass balance for the rectifying section. (From Smith R and Jobson M, 2000, Distillation, Encyclopedia of Separation Science, Academic Press reproduced by permission).

For the stripping and rectifying sections to become a feasible column, the two operation leaves must overlap. Figure 12.20 shows the system chloroform, benzene and acetone. The operation leaf for a distillate composition D intersects with the operation leaf for a bottoms composition... 

Weak nitric acid (normally 60 wt% HNO3) and concentrated magnesium nitrate solution (72 wt% Mg(NC>3)2) enter at the feed point of an extractive distillation column. The rectifying section above the feed point has a water-cooled... 

In a 500 ml. Pyrex round-bottomed flask, provided with a reflux condenser, place a mixture of 40 g. of freshly-distilled phenylhydrazine (Section IV,89) and 14 g. of urea (previously dried for 3 hows at 100°). Immerse the flask in an oil bath at 155°. After about 10 minutes the urea commences to dissolve accompanied by foaming due to evolution of ammonia the gas evolution slackens after about 1 hour. Remove the flask from the oil bath after 135 minutes, allow it to cool for 3 minutes, and then add 250 ml. of rectified spirit to the hot golden-yellow oil some diphenylcarbazide will crystallise out. Heat under reflux for about 15 minutes to dissolve the diphenylcarbazide, filter through a hot water funnel or a pre-heated Buchner funnel, and cool the alcoholic solution rapidly in a bath of ice and salt. After 30 minutes, filter the white crystals at the pump, drain well, and wash twice with a little ether. Dry upon filter paper in the air. The yield of diphenylcarbazide, m.p. 171 is 34 g. A further 7 g. may be obtained by concentrating the filtrate under reduced pressure. The compound may be recrystallised from alcohol or from glacial acetic acid. 

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... 

Fig. 4.12. Design diagrams for isopropyl acetate (IPOAc) reactive distillation column and comparison with simulation results (solid curves simulated column profile markers = stage composition for column rectifying section + = stage composition for column stripping section).

Referring to Figure 2.2 for MVC column configuration, the model equations for the rectifying section are the same (except the reboiler equations) as those presented for conventional batch distillation column (Type III, IV, V in section 4.2). The model equations for the stripping section are the same (except the condenser equations) as those presented for inverted batch distillation column (Type III, IV, V in section 4.3.2). However, note that the vapour and liquid flow rates in the rectifying and stripping sections will not be same because of the introduction of the feed plate. 

Figure 6.12 illustrates this effect. As more LLK component comes in with the feed stream, more depression occurs in the rectifying section temperature profile. If we control a tray temperature near the top and the amount of LLK in the feed increases, the temperature on this tray will start to go down. We will increase heat input to drive it back to its setpoint value, and this will push more HK component out the top. Therefore holding a constant temperature on a tray near the top of the column w ould result in significant variations in the amount of heavy key component in the distillate product. All of the LLK components must go out the top of the column, and there is nothing we can do about it once these components enter the column. Action must be taken in the upstream column to keep LLK components out of this column. Similar effects occur in the stripping section and near the base when variations occur in the amount of HHK components in the feed. Now temperatures rise as more heavy components enter the column, and we drop more LK component into the bottoms product if we hold a constant temperature on a tray near the base of the column. 

The entire rectifying section can be pressurized, and the heat can be transferred between any desired stages of the rectifying and stripping sections. This is called secondary reflux and vaporization (SRV) distillation. It reduces the consumption of both hot and cold utilities, and the sizes of the reboiler and condenser. However, capital cost is increased by additional intermediate heat exchangers moreover, since the process is more thermodynamically reversible, it requires more stages to achieve the desired separation. 

---