Entrainer in distillation

At higher vapor loads, the kinetic energy of the vapor rather than the bubble burst supphes the thrust for jets and sheets of hquid that are thrown up as well as the energy from breakup into spray. This yields much higher levels of entrainment. In distillation trays it is the most common limit to capacity. 

Anhydrous Acetic Acid. In the manufacture of acetic acid by direct oxidation of a petroleum-based feedstock, solvent extraction has been used to separate acetic acid [64-19-7] from the aqueous reaction Hquor containing significant quantities of formic and propionic acids. Isoamyl acetate [123-92-2] is used as solvent to extract nearly all the acetic acid, and some water, from the aqueous feed (236). The extract is then dehydrated by azeotropic distillation using isoamyl acetate as water entrainer (see DISTILLATION, AZEOTROPIC AND EXTRACTIVE). It is claimed that the extraction step in this process affords substantial savings in plant capital investment and operating cost (see Acetic acid and derivatives). A detailed description of various extraction processes is available (237). 

In the example, the minimum reflux ratio and minimum number of theoretical plates decreased 14- to 33-fold, respectively, when the relative volatiHty increased from 1.1 to 4. Other distillation systems would have different specific reflux ratios and numbers of theoretical plates, but the trend would be the same. As the relative volatiHty approaches unity, distillation separations rapidly become more cosdy in terms of both capital and operating costs. The relative volatiHty can sometimes be improved through the use of an extraneous solvent that modifies the VLE. Binary azeotropic systems are impossible to separate into pure components in a single column, but the azeotrope can often be broken by an extraneous entrainer (see Distillation, A7EOTROPTC AND EXTRACTIVE). 

Entrainment Entrainment in a plate column is that liquid which is carried with the vapor from a plate to the plate above. It is detrimental in that the effective plate efficiency is lowered because hquid from a plate of lower volatility is carried to a plate of higher volatility, thereby diluting distillation or absorption effects. Entrainment is also detrimental when nonvolatile impurities are carried upward to contaminate the overhead product from the column. 

In distillation towers, entrainment lowers the tray efficiency, and 1 pound of entrainment per 10 pounds of liquid is sometimes taken as the hmit for acceptable performance. However, the impact of entrainment on distiUation efficiency depends on the relative volatility of the component being considered. Entrainment has a minor impact on close separations when the difference between vapor and liquid concentration is smaU, but this factor can be dominant for systems where the liquid concentration is much higher than the vapor in equilibrium with it (i.e., when a component of the liquid has a very lowvolatiUty, as in an absorber). 

The heated oil is flashed into the VPS flash zone where vapor and liquid separate. Split between distillate and bottoms depends on flash zone temperature and pressure. Separation of vapor and liquid in the flash zone is incomplete, since some lower boiliug sidestream components are present in the liquid while bottoms components are entrained in the vapor. The liquid from the flash zone is steam stripped in the bottom section of the VPS to remove the lower boiling components. 

To obtain a low flash zone pressure, the number of plates in the upper section of the vacuum pipe still is reduced to the minimum necessary to provide adequate heat transfer for condensing the distillate with the pumparound streams. A section of plates is included just above the flash zone. Here the vapors rising from the flash zone are contacted with reflux from the product drawoff plate. This part of the tower, called the wash section, serves to remove droplets of pitch entrained in the flash zone and also provides a moderate amount of fractionation. The flash zone operates at an absolute pressure of 60-90 mm Hg. 

Slower introduction of the dinitrogen tetroxide, by either dropwise addition of an ether solution or entrainment in a slow stream of nitrogen, gave similar results. The direct injection method was found to be easiest. The checkers distilled dinitrogen tetroxide at atmospheric pressure (b.p. 21°) prior to use. 

Figure 12.33 Separation of isopropyl alcohol (IPA) and water mixture using di-isopropyl ether (DIPE) as entrainer in heterogeneous azeotropic distillation.

The VLB was also measured for binary and ternary systems of [ethanol + [C2Cilm][C2S04] and [ethanol + ethyl ferf-butyl ether + [C2Cilm][C2S04] at 101.3 kPa [151]. This ternary system does not exhibit a ternary azeotrope. The possibility of [C2Cilm][C2S04] use as a solvenf in liquid-liquid extraction or as an entrainer in extractive distillation for fhe separation of the mixture ethanol/ethyl fcrf-butyl ether was discussed [151]. 

The centrifugal supercontactor developed by Podbieiniak (46) is another fractionation apparatus in which centrifugal force is applied to the distillation process. The principal feature of the unit is a rotating spiral passageway which permits the employment of vapor velocities from 50 to 70 times greater than are possible without excessive entrainment in a bubble tray tower. 

The amount of entrainment has been studied mostly in distillation equipment. Figure 18.5 summarizes some of these data, and they are applied in Example 18.2. Equation 18.11 incorporates entrainment data indirectly. 

While the limiting phenomenon of upper limit flooding in a vertical pipe is similar to ultimate capacity in distillation, there is a distinct difference. Upper limit in a vertical pipe applies to a design where a conscious effort should be made to minimize gas-liquid contact. Carried to extremes, it would involve separate tubes for liquid flowing down and vapor going up. In contrast, ultimate capacity in a distillation column corresponds to the condition where effective mass transfer disappears due to high entrainment. One could force more vapor up through the contactor, but fractionation would be poor. 

The residence time is calculated based on the fluidizing gas velocity, assuming that the "free volume" (i.e. the volume of the expanded bed minus the volume of the sand) is fully utilized. At the temperature, total reactor gas flow rates, and sand bed volumes used, the residence time was about 0.5-1.0 sec. A typical operation began by washing the sand in 10% HNO3 and distilled water to remove impurities, such as iron, which may act as catalysts, and then calcined at 850° C for at least 12 hours to remove any sulfides and carbonates. The coal feed is then begun and pyrolysis products then exit the pyrolyser to a set of two cold traps fitted with cellulosic thimble filters maintained at 0° C. The outlet gas temperature after the first trap is 30-34° C. Much of the light char formed is entrained in the exit gas and carried into these traps, with most of it in the first trap. 

Because a large amount of water is entrained in the side stream, this is removed in the column C-3. Raw acetonitrile, namely a binary azeotrope with 20% water, separates in top. The bottom stream contains water with heavy impurities. Vacuum distillation at 0.5 bar is adequate to limit the bottom temperature. In the next step pure acetonitrile can be obtained by using pressure-swing distillation. 

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