ATCH Dit Introduction Batch distillation process has been growing in more applications in recent yeti, particularly in the production of specialty (fine) chemical, drugs, agricultural chemicals, etc, One of the simplest and oldest methods for the separation of miscible liquids is to put the mixture in a pot, bring it to a boil, condense the vapor, aiid collect the condensate in a séparate vessel. ‘The process is thousands of years old, but we call it Rayleigh distillation because Lord Rayleigh Gohn William Strutt, 1842-1919) derived the mathematics of thie process. ‘The process is beautifully simple and the mathematics aren't complicated, Unfortunately, however, Rayleigh distillation, (ie., one pot process) is not very useful inthe chemical industry because the compositions of both the distillate and the distilland change continuously throughout the process, and itis not possible to obtain either of them in pure condition. The Fractionating Column (Distillation Colunin): ne Imagine, if you will, a whole series of Rayleigh distillations. Vapor from the first pot passes into the second pot where it condenses: The heat of condensation causes the second pot to boil and this vapor passes into a third pot. ‘This process can be repeated for as many pots as one wishes. Since the vapor from each pot is richer in the more volatile component than the vapor from, the preceding pot, itis apparent that any degree of vapor purity can be obtained simply by increasing the number of pots. While the vapor is being transferred from pot to pot in one direction, let us transfer liquid from pot to pot in the other direction. This avoids accumulations and depletions along the line. In order to maintain the process it will be necessary to ietim some condensate, from the last pot to the system, ‘This hypothetical combination of a number of Rayleigh distillations in series is the essence of the fractiondting column. Each plate, or tray, of the column is a litle Rayleigh distillation pot. Tt is convenient to arrange the trays in sequence vertically so that the liquid flows downward by gravity and the vapor flows upward. Vapor and liquid mix intimately on each tray. Oné way to bring the liquid and vapor into intimate contact is to force the vapor to.rise through a layer of liquid in the form of fine bubbles. As liquid flows down the column it flows across a tray, qverflows into a pipe called a downcomer, and then down to the next tray. The top end of the downcomer projects above the surface of the tray so that some minimum depth of liquid is Maintained. ‘The bottom of the downcomer is submerged in the liquid on the tray below so that vapor cannot flow up through the downcomer as shown below. PPpopespe ee Gas flow a ) Liguid flow \ FIGURE 172 Seve plate: , tray or plat: B, perforations: C, downcomer to plate below; D downcomer from plate above, ;‘Vapor rises through holes in the tray, mixing with the. liquid as fine bubbles. Fine bubbles are created in various ways. ‘The simplest design is the sieve tray. The tray floor is merely a large piece of wire screen, or a metal plate with small closely spaced holes. Vapor flows up through the holes. It flows upward fast enough that liquid doesn't leak down. Af least, liquid doesn't flow (‘weep") through the sieve in significant amounts when the column is operating under design conditions. This is onc of the problems with sieve trays: too high a vapor flow rate and the column floods; too low a vapor flow rate and the trays weep. Sieve trays have a very narrow range of operating conditions between flooding and weeping. Another Kind of tray has large holes for vapor, each with a short section of vertical pipe which creates a dam around the edge of the hole. The dam around the vapor hole Keeps the liquid on the tray from bypassing through the hole into the tay below. It cannot go anywhere except across the tray to the downcomer. The vapor tising through the holes is deflected downward by. a cap and escapes from under the edge of the.cap to rise as bubbles through the liquid on the tray. Setrations or slots on the edge of the cap enhance the formation of smell bubbles. This is called a bubblecap column. Since liquid cannot flow down through the vapor holes, but can leave only through the downcomer, it is apparent that the column can maintain a good liquid level and operate successfully over a wide range of vapor velocities. ‘Turndown ratio is the ratio between the maximum and minimum boilup rates possible while maintaining good operating conditions. Too high a boilup rate causes the column to flood. Too low may réduce the effectiveness of the separation. A bubblecap column is said to have a good turndown ratio because it operates well over a wide range of boiling rates. On the othor hand, it is a good deal more expensive to construct than a sieve tray column, Still another kind of tray, called a valve tray has many holes, each closed with a little plug that lifts when there is sufficient pressure from the vapor below. Bubbles then escape through the liquid on the tray. ‘This kind of tray has the advantage of requiring less liquid on the tray than the bubblecap column, which may mean better contact between liquid and vapor. It has a better tumdown ratio than a sicve tray because weeping is not a problem. The bubbles, however, may ‘hot be as fine as we would like, and the valves may not all operate efficiently. Another kind of tray is the ballast tray. It is a combination of the bubblecap and the valve tray. I is like the bubblecap in that in operation the vapor comes up through a hole and is déflected R= (28) recalling equations (23) and (26): et, Lo DPE TD @) - *e Xp pn Rt Real (26) By substituting D = 0 or Ry = o» in equation (23) or (26), respectively, yields: Maar = % +0 where the slope is 1 (Le. the diagonal) and the intercept is 0 (i.e, the origin of the diagram). Minimum Number of Plates: At total reflux (R, =<) the required mimber of plates for a given separation is at a minimum. ‘Therefore, total reflux represents one limiting case in the operation of the distillation column. ‘The minimum number of plates can be found by constructing steps (McCabe-Thiele diagram method) on an x-y diagram between compositions xp and x, using the diagonal (i.e. 45_ line) as the operating line. Minimum Reflux Ratio: At any reflux Jess than total, the number of plates needed for a given separation is larger then at total reflux and increases continuously as the reflux ratio is decreased. As the ratio becomes smaller, the number of plates becomes very’ large, and at a. definite minimum, called the ‘minimum ceflux ratio, the number of plates becomes infinite. For any xy (bottom composition), the minimum reflux ratio can be.calculated using: ~ A spreadsheet program provided to the students by the TA ‘The following equation and/or McCabe-Thiele diagramOperating Line of a ‘minimum reflex ratio (Roy) slope Row ‘The slope of the operating Line is Solving this equation yields: Plate Efficiency: ‘To translate ideal plates into actual plates, the plate efficiency must be known. The following are the three kinds of plate efficiency used: i, Overall efficiency or column efficiency (7,): It is simple to use but is the least fundamental. The overall efficiency which concems the entire column, is defined as the ratio of the number of ideal plates needed i an entire column to the number of actual plates, For example, if 6 ideal plates arc called for and the overall efficiency is 60%, the number of actual plates is 6/0.6 = 10 number of idealplates 19) number of actual plates ii, Murphree efficiency (7,,): Murphree efficiency, which has to do with a single plate, is defined by 10! = Ss Ny, = A—H*2 x 100 Ya ~ Yao where y, actual concentration of vapor leaving plate 7 Jeet = actual concentration of vapor entering plate n % concentration of vapor in equilibrium with liquid leaving downpipe from plate n Local efficiency (1) ): Local efficiency, which pertains to a specific location on a single plate, is defined by Yor’ = Ye—MHw+L x 100 Yen Fav where yf = concentration of vapor leaving specific location on plate n Yee = Concentration of vapor entering plate at same location Yon = Concentration of vapor in equilibrium with liquid at same location Since y; cannot be greater than yZ, , a local efficiency cannot be greater than 100%. iz, Is Mode of Operation for the Batch Distillation Batch distillation can be operated in two modes of operations as follows: ‘The top composition is kept constant by increasing the reflux ratio. ‘The McCabe-Thiele diagram for this mode would have operating lines of different slope (i.c. Rp #1 Pinses) positioned such that the same number of ideal stages was used to go from %p to X, (the bottom composition) at any time. A typical diagram is shown in the figure below Figure 18-36) for a batch distillation with five ideal stages including the reboiler. ‘The ‘upper operating line is for the initial conditions, when the concentration of low boiler in the batch distillation column is about the same as the charge composition (The concentration x» is slightly lower than ~, (the initial) because of the holdup of liquid on the plates). ‘The lower operating line and the dashed line steps show conditions when about 1/3 of the charge has been removed as overhead product. Determination of the reflux needed for a constant x, and given x» requires a trial-and-error calculation, since the last step on the assumed operating line must end exactly at xp. However, once the initial reflux ratio is chosen by this method, the value of x, for a later llstage in the distillation can be obtained by assuming a value of Ro, constructing the operating line, and making the correct number of steps ending at x,. By the following balance, the amount of product and remaining charge can be calculated. F Product: D Fx; Component A: Dxp Remaining in the reboiler: B Component A: Bry ‘Total material balan¢ Initial charge = product + remaining F=D+B 29) Component A: Pap = Dp + Bxp 0) FIGURE 1836 McCabe-Thiele diagrams for a batch distillation. Upper operating fine and solid lines: initial conditions; fower operating fine and dashed lines: afer onethird of the ‘charge bas been removed. 12‘The reflux ratio is fixed and the overhead product purity is varied with time. An alternative method of operating a batch distillation is to fix the reflux ratio and let the overhead product purity vary with time, stopping the distillation when the amount of product or the average concentration in the total product reaches a certain value. Hence, in this mode of operation, the compositions of both the product and the still change with time and therefore the boiling temperature in the still changes with time too. Accordingly, the following calculation can be performed: (to calculate the performance of the distillation column, operating lines of constant slope are drawn starting at each new value of x, and actual number of stages is stepped off to determine Xp, (2) If x, can be measured, the number of stages between x, and x, measured at the same time can be calculated using McCube-Thiele diagram, Such number can be compared with the actual number of plates and the overall efficiency of the column can be determined by no. of plate (McCabe-Thiele diagram) — 1 thane = Tent actual number of plates Gh where the actual number of the plates in the column is 8 excluding the reboiler. It is noteworthy to mention that the number of plates evaluated by McCabe-Thiele diagram includes the reboiler if you measure reboiler concentration (%)- ‘Therefore, 1 is subtracted from the numerator of eq.(31). However, if you take a sample from the bottom of the column (stage no. 1), there will be no need to subtract from the calculated no. of stages. (G) Ata certain moment or time, the total number of moles left in the still can be calculated provided that xp and xp are either measured or calculated with time between the starting time and the moment or the time at which the number of moles left need to be calculated. In other words, the following table of data is required: ~_ | Total number of Time | Bottom Composition | Pr oduct Composition moles left te Xap on Ty 4 Ea Fo. ty ny? 3By integrating eq. (4), the total number of moles left (n,) can be determined numerically. 2) where yin eq, (4) is equal to xp since the evaporated vapor is condensed and collected as a product with a composition of xp, and x (of eq. 4) is equal to x, (the composition in the reboiler) 14—_— aS SSS * Additional Background Other computations which must be made to satisfy the assignments of this experiment are as follows: * Heat lost from the entire system operated under total reflux to the ambient By neglecting Que ince CWHY?), Qiay Can be estimated as follows: Qrea = Qin eriery ~ Qos coder Qreoron =P Tae ~ Typ) ‘The physical properties (such as cp) can be evaluated at the average temperature between the inlet and the outlet temperatures. NOTE: Qoeonnace WoUld be approximated or estimated based on empirical approach since there is not enough information to measure it, a ‘Heat lost from the system operated under a certain reflux ratio to the ambient. Jn this case you need to account for the enthalpy of the product stream based on a reference temperature. 15** Feat lost from the column to the ambient by natural convection (Welty et al., 1984). The following steps are necessary to evaluate the heat lost from the column only: to the ambient by natural convection. a heat L 1. Assume the wall temperature (glass) equal to the liquid tos temperature (ie. neglecting inside film resistance). 5 2. Take the wall temperature as the average temperature between plate L.to 8. 1 3. Neglect the resistance to heat transfer through the glass wall. Accordingly the heat lost can be determined 44 - | ( Qesten, ~ PAG - T.) i insulation where, A, is the outside surface area of the insulation surrounding the column. NOTE: Measure the insulation thickness. The insulation material is glass wool. In this case, assume constant outside diameter of the insulation along the column by neglecting the insulation around the flanges used to mount the trays (or evaluate the average outside diameter by including the outside diameter of the insulation around the flanges) as shown below the outside diameterto | [‘¢—]— bbe considered ae ae neglect this part fr account forit oe by taking the verge 16: (Welty, et.al, 1984, page 237) or (ses the heat transfer coefficients experiment) 4s is neglected by assuming the glass wall temperature equals to the temperature of the liquid inside the column. Aj: Tr: Ty, Land & are known (the thermal conductivity, k, would be found from the literature based on the type of the insulation - glass wool or equivalent materials). A, (outside natural heat transfer coefficient) now is needed which can be calculated based on the natural convection given by Welty, et. al., 1984, page 357 as follows: Calculate Gr, where L refers to the axial length of the column, Gr: Grashof number Bg p* 2 AT/p” Bg p"| u? jis found for air from Appendix I (Welty ét. al., 1984). Physical properties ‘Would be’evaluated at the average temperature, AT = T, - Tow = Check for 35 L ari* If this is achieved then Nusselt number, Niy,, equations for vertical plane surfaces can be used where the curvature effect is not too large. If the above relation is not achieved, the curvature effect of a vertical cylinder is too large and error would be associated in using vertical plane surfaces equation. Thus, the results should be discussed accordingly. = Caloutate Re J Ra = Pr Gr 213 Re: Rayleigh number = £2, are Pr: Prandd number yar = pLep/k If Ra > 10? , use the following correlation iGio Nu, = fos + 0387 Rai | [b+ (eas2eny] If Ra < 10°, use the following correlation us Nu, = 0.68 + ——2et Ray i + (0.492yP1)"*] | where (jVu,) Nusselt number = a Accordingly, h, is calculated : NOTE: Heat lost from the column can also be obtained as (where the heat added by the steam trace is not accounted for): Heat lost from the column = (heat lost from the entire system) - (heat lost from the reboile:). ‘This can be compared with that obtained by natural convection calculations mentioned above. Internal Reflux Rate In a distillation column, there is always some intemal reflux (i. extra condensation inside the column) due to the loss of thermal energy from the column to the ambient. In large commercial columns this is only a small fraction of the external reflux (R,) while in small pilot plants or laboratory scale columns (e.g. lab experimental column) it may be significant. ‘The internal reflux rate is estimated as follows: © Volumetric flow rate of the internal reflux vemal = Oxrean rom ~ Qrghuxsiom = Qt, votom ~ Or, re fees ese te Geel nee Ls ‘oteralar where Q, ton Ad Q,, em, Can be measured using the rotameter on the liquid outlet stream from the column to the reboiler and the rotameter on the reflux stream from the condenser, respectively. Mass flow rate of the internal réflux The stream from the bottom of the column to the boilier is sich with the heavier component (TCE), while the reflux from the condenser is rich with the lighter component (MC). Sampling these streams enables estimating the’ mole fraction of each component, where average density can be calculated as: 18= Puc*uc + Pice Frc ‘Knowing the average density of each stream, you can-convert the volumetric flow rate into mass flow rate. Hence Mirsernat = Mr, bouom reflec Mi, retes Beat lost to the ambient due to the condensation of the internal reflux Dyas = (Ablags MC) (Mey vata) tctatee ~ Mies az) thay TCE) (rex tam ~ Mr.) ‘Heat of evaporation should be estimated at the average temperature using Table 4. Energy balance on the condenser: Heat taken by the cooling water and heat given by vapor condensation Heat taken by cooling water = heat given by vapor condensation. R super heated MC & TCE column water col Heat taken by cooling water = 0, = mep (r Sat Tan) aE Heat given by vapor condensation = heat given by MC condensation + heat given by TCE condensation Based on areference temperature, Heat given by MC condensation = [Mycop Cv BPyc)la, + Myc Atay, we * [Muco? (BPuc ~ T., 19.Heat given by TCE condensation = [Myce cp (Ty — BPrce ap + Myce Sap, rce + [Mrce ©? (BPree ~ Ty, where BPyc and BP;oe are the boiling points of MC and TCE, respectively. 20— = = = mn mane a =| Equipment Description ‘The system consists of a glass fractionating column with a condenser and reboiler, two tanks, pumps with associated piping, a heating system which can use either circulating heat transfer fluid or steam, and a computer data-logger. For casy illustration and understanding the system is shown as three inter-related sub-systems: Figures 1, 2, and 3 show the arrangement of the piping, valves, pumps, sample points, etc., that must be known to operate the column, Fig. 1. Column System Fig. 2. Reboiler, Pump and Tank Sysiem Fig. 3. Heating System The liquid to be distilled is a mixture of cominercial grades 1,1;1 trichloroethane (MC, Methyl Chloroform) and trichloroethene (TCE). Physical and transport properties of the substances are given in Tables 3 and 4. Properties are copied from reliable sources (Smith and Srivastava, 1986; Reid ct al., 1987; Perry, 1984). Where data were not available, properties were estimated, of extrapolated into the needed range, using standard methods (Reid et al., 1987; Perry, 1984; Smith and Van Ness, 1987). In the absence of heat-of-mixing data we can assume the mixture properties are additive. Since the infinite dilution activity coefficients (as estimated) are very sinall, the assumption is justified. The column has cight plates plus a reboiler. Each is a metal ballast tray (Glitsch type V6, with three V6 units per tray, as shown in Fig. 4) clamped between sections of glass pipe. As described ceatlier, the trays operate like valve trays, in that they open in responsé to pressure from below, but on opening they behave more like bubble caps. A skirt directs vapor flow dowaward into the liquid. ‘The trays are clamped between sections of glass pipe, each 6 inches inside diameter by 8 inches long. ‘There are two glass sections between each tray so that the tray spacing is 16 inches. -The joints between the sections and the trays are sealed with teflon envelop gaskets and are held together with bolted clamping rings. ‘Thus the joints are resistant to solvent or chemical action, and cai be ‘maintained tight by adjusting the clamping pressure. There is a 1-inch diameter downcomer between trays. There is a thermocouple, for temperature measurement, in the liquid on each tray, except for the top tray where the thermocouple is in the vapor space. Plates are referred to by numbers, starting with number 1 at the bottom. ‘The reboiler is a horizontal cylindrical tank, 19.5 inches inside diameter by 34, inches long (Shoilder to shoulder - the overall length would include two dished heads, cach 3.5 inches deep). ‘The inside area of the reboiler is ~20.5 12, The walls are 1/16 inch thick. The reboiler is made of admiralty rietal. It is provided with a pressure relief valve, a mercury manometer to indicate pressure, and a liquid level gauge. ‘The reboiler is heated by three sets of coils, each consisting of three hairpin tubes, 0.625 inches O.D. and have walls 15 BWG (Birmingham Wire Gauge, where 15 indicates 0.072 in), extending 36 inches horizontally into the reboiler. (The tank opening through which the tubes are inserted projects about four inches from the end of the tank). ‘The center-to-center distance between the legs of the hairpins is sbout four inches. The coils lie within the space between the. bottom of the reboiler and six inches above the bottom. The outside area of the heat transfer coils is 1313 in®. Their total length is 669 inches. Their contained volume is 121.6 in?, Their internal cross-sectional area is 0.1817 in, 2‘The reboiler can be heated directly by steam. For the liquids currently distilled, better control is obtained using heat transfer fluid. ‘The fluid is a solution of 65% by weight, ethylene glycol in water, It is heated to 2 constant temperature and pumped through the heating coils using the heating system shown in Figure 3. The flow rate is indicated by a rotameter, and the temperature of the fluid in and out is indicated and recorded by the data logger. ‘The reboiler pump takes liquid from the reboiler and will transfer it either to the product or to the feed tank. The product pump will transfer liquid to the reboiler or the feed tank. ‘The condenser is a single pass shell-and-tube heat exchanger, mounted vertically. "Vapor and condensate are on the tube side, which is vented to the atmosphere at. the outlet, ‘The column therefore operates at atmospheric pressure. Water enters the shell side at the boftom and leaves atthe top. The heat exchanger contains 26 tubes, 3/4 inches O.D. by 5/8 inches LD. by 36 inclies long, made of stainless-steel. PERE ‘The splitter.is an electrically operated valve, The position of the valve is controlled by a solenoid. Tn one position condensate is retuned to the column as reflux.. In the other position condensate is diverted to the product tank. The solenoid is actuated by a Flex-Pulse. timer mounted on the control panel. ‘The operator sets the amount of time desired for each part of the cycle. A lamp bulb near the solenoid lights when the solenoid is actuated to withdraw product. Tn setting the Flex-Pulse timer, it is recommended that only short periods of time be used (5 or 10 seconds for the shorter part), to minimize disturbances to the column, ‘The feed tank contains the mixture to be distilled. It is a vertical stainless steel cylinder, 35.75, inches inside diameter by 48 inches high, with a hinged lid and a level gauge. ‘The product tank is identical to the feed tank in construction and dimensions. Both tanks have sealed lids and are vented to the atmosphere at a point near the ceiling of the laboratory. Any escaping vapor will be carried away by the ceiling exhaust fan. ‘The process piping is of copper thing with solder-sweated joints, almost entirely. The steam lines are iron, with screwed fittings, and the water lines-are brass, with screwed fittings. Flow rates are indicated by rotameters. Rotameters aie calibrated for water, which bas a specific gravity of 1.0 and a viscosity of 1.0 centistoke. Reasonable variations in viscosity (up to 20-centistokes) of the fluid through the instrument do not have a significant influence on’ the indication. The density of the fluid measured, however, affects the flow indication. The reading is a balance between the upward force of the flowing liquid and the downward force of gravity acting on the float. ‘Therefore to obiain the true volumetric flow rate the indicated rate must be corrected as mentioned in the introduction section. In a denser fluid the downward force of the float is less. The rotameters have calibrations as shown in Table 1, based on water flow, for 100% full scale, All rotameters are mounted on the instrument panel; except for the overhead condensate rotameter which can be observed from the second floor balcony, and the heat transfer ‘fluid rotameter which is mounted on the heater apparatus. Rotameters are most accurate in the upper 80 percent of their flow ranges. Where possible, flow should be set to that part of the range. 2Table 1 ROTAMETER CALIBRATIONS Heat Transfer Fluid Feed Tank to Reboiler Product Tank to Feed Tank Flow Indicato Reboiler to Feed or Produc! Flow Indicator * Condenser Water 1.12 gpm full scale fidensate to Splitter Retur to Reboiler Bo *A rotating element indicates only the flowing of the fluid. ‘Table 2 DATA LOGGER INPUT LIST 1 Heating Coil in 2 Heating Coil out 3 Reboiler Vapor 4 Plate 1 5 Plate 2 6 1 8 9 Plate 3 Plate 4 Plate 5 Plate 6 10 Plate 7 i Plate 8 12 ‘Vapor from Plate 8 B Vapor to Condenser 4 Condenser Water in 15 Condenser Water out 16 Condensate to Splitter 23‘Temperatures are measured with copper-constantan thermocouples, connected to a computer data logger. ‘The thermocouple channels are identified in Table 2. They are polled every.two minutes and the current Values displayed on the computer screen, They are also printed, giving a continuous written record, and can be recorded on 2'3 1/2 inch floppy diskette as well. The operating controls are on the control panel. ‘The main electrical switch is mounted at the right edge of the panel. It is closed by raising the red-insulated handle, Individual switches control power to the pumps, and to-the Flex-Pulse timer. They are turned on by pulling the switch knob toward you, When the switch is oa, a red pilot light in the knob glows. Valve handles controlling individual flows extend from the panel board beneath the flow indicator for that stream. Valves not on the panel board can be found with the help of the flow diagraths, Figs. 1,2, and 3. Analysis of overiiead and bottcms liquids is performed by either refraction index or Gow-Mac ™ gas chromatograph, series 550; with thermial conductivity detector. (Gow-Mac listrument Co., Bridgewater NJ, USA). The Gas Chromatograph is provided with a Spectra Physics SP4270 Integrator, which graphs the peaks and reports the integrated area under the peaks. Each peak indicates a component of the sample, and the area under the peak is proportional to its volume fraction in the gas phase, That is, the area of the peak is proportional to the mole fraction present. NOTE: If you are not familiar with the chromatograph, get instruction before trying to use it! In addition to the peaks for 1,1,1 trichloroethane (at about ~2.5 minutes) and trichloroethene (at about ~3.5 minutes), you will observe several small peaks, both before and after the main peaks, indicating the presence of other substances. These are inhibitors, For our purpose these minor ingredients can be ignored, Normalize the results for the two major peaks.Oper: jure At the start of the distillation, operate the column at the total reflux with a boilup rate such that the pressure drop through the column is about 1 to 2 inch Hg. The vapor which initially comes from the liquid in the still pot is in equilibrium with the liquid charged. It can only be enriched to the desired product concentration by bringing it into contact with liquid reflux which is itself tich in the more volatile component. ‘The initial concentration in the condensate retuned to the column will almost ceztainly not be rich enough. Also, it takes time for the trays to fill to the normal operating level with liquid. Operation at total reflux is continued until distillation conditions are-at a steady state. At this point the overhead will have (presumably) reached or exceeded the desired concéntration of the more volatile component’ Data for the energy balance can then be taken. ‘The reflux ratio can now be set to the value necessary to maintdin the product concentration at or above some specified level. (A spreadsheet program -available:on the laboratory computer enables this to be determined very quickly. ‘The properties of the mixture to be distilled are already loaded into the program). As the bottoms composition changes with time, two modes of operation are possible. a, Maintain a constant reflix ration, This results in variable product composition. By this method it is possible to separate a given reboiler charge into a numbér of successive distillate cuts, each having an average composition less rich in the more volatile component than the previous cut. . If a distillate of a particular composition is desired, it is necessary to increase the reflux ratio as the bottoms become depleted of the more volatile component. ‘This results in a decrease in ‘output until finally the productivity is minimal and no more of the more volatile component can be removed profitably. Frequently, a combination of these two methods is used. 25ASSIGNMENT OBJECTIVES: You are requested to define focused objectives for this experiment which represent the task(s) (ie., the assignments) to be performed. NOTE: _ The purpose of the enclosed list of assignments and discussions is to provide you with guidance and ideas. It is not meant to be followed as is nor to propose an equivalent amount of work. You may define only one objective or one task that, based on its results and findings, you can give the reader an important message that reflect the purpose of the experiment. PURPOSE: Ina separate subsection you will need to state, based on your. defined objective(s), the purpose of the experiment which poses the problem to be solved and the scope.4 v ! Assignment ae ! For pre-Lab proposal, create flow diagram (P&ID - Process Instrumentation Diagram) showing 1 process etc.). SI TI Ss ies, components, instrumentation, etc., comectly labeled (ie. values type, pumps type, VI CI Y G E Operate the batch distillation column at total reflux and stale. Steady state is obtained when the temperatures and the column presstre repfain relatively stable (unchanged Significantly) with time (~1 to 1 1/2 hours). Since the pélumn is at total reflux, the vapor rate exiting the column is the same as the reflux rate enteying thé-column, in moles per unit time. Heat loss from the column can be estimated by three different methods given-in (1), (2) and (Bb) below. ~ x I slimate the heat lost from the system to the ambient ased-on overall heat balance (the heat loss from the reboiler using the heat transfer coefficieit obtained in.experiment (2)) 2. Determine the heat lost-froiii the column only to the ambient by natural convection. Compare and discuss the value with that obtained in (11) above. Is the natural convection correlation suitable? If not, suggest other alternatives. V3, a, Botimats the overall volumetric and mass rte of the internal reflux. b. Estimate the heat lost to the ambient due to the condensation of the intemal reflux estimated in (a). ©. Compare the heat lost obtained in (b) with those obtained in (12) and 4. How does the intemal reflux affect the operation and the performance of the distillation column, Evaluate the minimum number of stages required to achieve the steady state mole fractions of the MC compotind (i.e. x, and x,). Show yout calculation on McCabe- Thiele diagram, 5. Estimate the column efficiency (overall plate efficiency). Discuss’ the obtained value baséd on the results obtained in (1), (2), (3), and (4) above, Is the McCabe Thiel Diagram calculation suitable for the present experiments. Discuss alternatives. 6. Estimate the minimuin reflux ratio needed to achieve the steady state mole fractions of the MC compound (i.e. x, and x,). What is the number of plates required at this tminimum reflux ratio? Show how do you obtain these values on McCabe-Thiele diagram. 7. Estimate the composition of the liquid inside the reboiler by the following: 26 Caneri, xp is evaluated by using McCabe-Thiele diagram, starting at xp and using the actual umber of stages (8 + 1 of the reboiler = 9), ii, 2p is estimated by measuring the boiler temperature and using T-x-y diagram where the vapor and the liquid are considered to be in equilibrium. ‘Compare the obtained values of x, above with that measured using the analytical equipment (GC or refractive index). Operate the batch distillation column under the unsteady state mode where the reflux ratio is fixed, and the overhead product purity and the reboiler compositions are varied with time. In this case, set the reflux ratio at twice the minimum reflux ratio obtained in (16) above. For the remgiing time in the laboratory, continue g, using the set value of the reflux ratio (Re, “ie ‘and the heating fluid temperatures without further adjustment. 18 1 aNSiom the time dependence of the liquid compositions (MIC and TCE) of the overhead (product) and the reboiler. b. Show the time dependence of the volumetric flow rate of the overhead (product) and the liquid stream from the bottom of the column to the reboiler. Disctiss and explain the results and the trend for this operating mode. 2. Ata time toward the end of the operation, do the following: a, Measure the total number of moles left in the reboiler. b. Calculate numerically the total number of moles left in the reboiler (as discussed. earlier). Compare between the values obtained in (a) and (b). Discuss the difference if any. 3. Select two sets of measure data (x, and x,). One set’at a time toward the beginning of this operating mode and another set at a tinie toward the end of this operation. - Bvaluate and show for both sets separite McCabe-Thiele diagram, the number of plates requiréd.to achieve the compositions (xp and x,) and evaluate’ the overall column efficiency. - What would be the minimum reflux ratio for each set of data? Show the minimum reflux ratio operating line on the McCabe-Thiele diagram. Compare the results of the two sets of data with each other and with the results obtained in (1) above (ic. total reflux operating mode). 27ae i i Results and Data Analysis Outline Present the direct and indirect results that represent the assignment in the form of equations, number, tables and figures. Meanwhile, provide interpretations of the results (ie. provide a thorough and concise discussion of the findings). The results should be discussed in the light of ‘uncertainties of measurements (i. identifying the sources of the experimental errors, are these errors significant? Their impact on the data and the calculated results, etc), stalistical analysis of the experimental data, significance and meaning of any calculated numbers, trend of the data and the results, etc. Data analysis may include, but is not limited to; the following discussion outline: Assignment I: 1. Discuss the value of the heat lost to the ambient. Is it large or reasonable? Explain. Through Which parts of the process does the heat loss occur. To what extent, does the error in your measurements affect the obtained value of the heat loss, etc. 2. Discuss the calculation steps and the possible errors associated with evaluating the heat loss from the column to the ambient by natural convection. How big is this value compared to that obtained in 1? What does this tell you? ‘Explain. 3. a. Define the internal reflux. Is the internal reflux large or small. Explain why? b, Discuss and compare the value of the heat loss to the ambient due to the condensation of the internal reflux to that obtained in (2). Explain the relationship between the internal reflux and the heat loss from the column. ©. Explain how the intemal reflux can be minimized. Is it better to have internal reflux or to climinate it or to minimize it? What are the advantages and the disadvantages of the internal reflux? Explain how the internal reflux affects the performance of the column. Does the internal reflux change along the column? Why’ 4. Discuss the evaluation of the minimum number of plates and the overall plate efficiency. Are these values reasonably large or small? Explain why? 5. Define the minimum refiux ration (Rp,)- Discuss and explain the estimation of the Ro, How accurate is your estimation? 6. Discuss how to calculate the compositions of the liquid inside the reboiler and compere the value with that obtained experimentally using the available analytical equipment. Explain the differences if any and state why. 28Assignment I: State the advantages and the disadvantages of this operating mode. Explain briefly what is happening when the column is operated under such mode. 1. Discuss and explain the time dependence of the compositions and the flow rate.. Is the observed trend consistent with the trend of this operating mode? 2. Ts the measured value of the moles left in the reboiler at the end of operation close to that calculated numerically. Discuss the results and the differences. 3. Compare the estimated number of plates, overall efficiency and the minimum reflux ratio between the two sets of data that you have selected. Discuss and explain the differences. Is the slope of the operating line constant for both sets or not? What does this mean? Should the number of plates and overall efficiency be similar in both sets or not? Why? Are these values close or not to the values obtained at total reflux operating mode (Assignineat 1). ‘What should it be (similar or not)? Explain why? 29ga 2 & & = References L ‘MeCabe, Warren L., Smith, Julian C., and Harriott, Peter, "Unit Operations of Chemical Engineering", Sth ed., New York, McGraw Hill Book Co. (1993). Gilland, ER., "Elements of Fractional Distillation", New York, McGraw-Hill Book Co., 370-383 (1950). Block, "Chem Eng.", 68, 88 (Feb. 6, 1961). Bogart, “Trans. Am. Inst. Chem. Eng.", 33, 139 (1937). Smith, Buford D. and Srivastava, Rakesh, "Thermodynamic Data for Pure Compounds, Part V, Halogenated Hydrocarbons and Alcohols", New York, Elsevier (1986). Reid, Robert C., Prausnitz, John M., and Poling, Bruce E., "The Properties of Gases and Liquid", 4th'ed., New York, McGraw-Hill Book Co. (1987). Green, Don W., editor, “Perry's Handbook of Chemical Engineering", 6th ed., Section 3-137 to 3.278, New York, McGraw-Hill Book Co., Inc. (1984). ‘Smith, J.M. and Van Ness, H.C., " Introduction to Chemical Engineering Thermodynamics", 4th ed., New York; McGraw-Hill Book Co. (1987). 30Table 3 Properties of Components in Mixture Chemical name 4,1, 1-Trichloroethane Trichloroethene Common name Methyl Chloroform, Trichloroethylene (Abbreviation) acy (TCE) Molecular formula CLC.CH, CLC:CHCL Index formula C2H3CI3, C2HCI 7) Molecular weight 133.41 131.39 Density liquid, @ 25 C, g/cm? 134 1.45 Meltitig point, C -33.15 86.35, Boiling point @ 760 mmig, C TAI 86.90 Critical Temperature, 545.00 572.00 Critical Pressure, bar 43.00 50.50, Critical Volume, om’/gmol 256.00 ‘Critical compressibility, Z, 0.27 Pitzer’s acontric factor 0.22 021 Viscosity, liquid, @ tibp, es 0.26 0.26 ‘Therm.cond.@ 0.08 0.08 50 C, Bey (hrf FIA) Flash point none none + =) | Antoine constant A* 6.81 714 Antoine constant B* 1148.90 1430.40 Antoine constant C* 218.35 249.08 >| Inf. Dil. Activity Cost. 1.109 1.075 Enthalpy of vap'n @nbp, cal/gmol 7096 716 Htcap.liq @ 20 C, cal/(g C) 0.266 0.223 aLa oe t 4 Table 4 Component Properties in the Boiling Range 1.1, Mrichloroctiane (MIC) ‘tichloroethene (TCE) t 1 pt lep.tig Cpo, gas fRnowig | Hv | pt [Cp.tiq Cpo,gas,|Rhowig | Hv deg.C |ombig | cal(gmol.c) | pfem3_fal/gmot | mig |” caligmotc) | wema_{cavimot 70-6687: | 339 | 2298 | 1.256 |r1s17 | 4523 | 312 | 2049 | 1.377’ |739.4 n1_| e902 [339 | 23.02-| 1.254 |rae4 | 67a | 312 | 2051 | 1395 [73199 m_| 723 | 340 | 23.06 | 1253 [71249 | 4823 | 312 | 2054 | 1373 [7104 m_|7349 | 340 | 23.10 | 1251 |r| 4979 | 313 | 2056 | 137 |73010 74_| 758.1 | 361 | 23.14 | 1.249 {70978 | 5139 | 313 | 2059 | 1369 [aa914 75_| 71.8 |'361 | 23.18 | 1.208 [70842 | sa04 | 313 | 2061 | 1367 [7281.9 16_| 8062 | 341 | 23.29 | 1.246 |ro705 | 5412 | 313 | 2068 | 1365 [72724 m_|s31.1_| 342 |23.26 | 1245 |70567 | seas | 314 | 2066 | 1363 | 72628 7s_|.8366 | 342 | 2330-| 1243 |70a28 | 5x22 | 31.4 | 2069 | 1361. [72532 7 _|'s27 | 343° | 23.34 | 1241 |7org9 | 003 | 314 | 20:71 | 1339 [7203.6 80_| 904 | 343 | 2338 | 1240 {7015.0 | 6189 -| 315 ‘| 2074 | 1357 [7234.0 s1_“|9367 | 344 _| 23.42 | 1.238 [70009 | 380-| 315 | 2076 | 1355_|72203 82_| 9647 | 344 | 2345 | 1237 Jones | 6575 | s15_| 2078 | 1353 [72146 s3_|.9933 || 345 | 23.49 | 1235 |6072.7 | 77s | 316 | 2081 | 1351 [72049 84_|1022.6 | 346 | 23.53 | 1233 loose | 6980 | 316 | 2083 | i349 [71952 85__|10525 | 346 | 23.57 | 1.232 |oos41 | g9-| 316. | 20.86 | 1347 [71855 86__|1083.1 | 347 | 23.61 | 1.230 }od2927 | 1404 | s17_ | 20.88 | 1345. [7175.7 87_|ind4 | 347 | 23.65 | 1.229 |oo1sa | 7624 | 317 | 20.90 | 1343 | 71659 se_|in463 | 348 | 23.69 | 1227 [69008 | 7349 | 31.7 | 2093 | 1341 |71569 s9_|1179.0 | 348 | 23.73 | 1.225 168862 | soro | 31.7 | 2095 | 1339 [71463 90 _|i2i24 | 349 | 23.77 | 12974 |osms | saa | 318 | 2098 | 1337 [7365 32Table ‘Heat Capacity of Ethylene Glycol in Water ~~ in calf(g 6) or Btu/(lb,°F) Temp. _C \., Ethylene glycol, percent by weigt@ ro | so St 60 40 20 10 10 0556 | 0653 | Sars | ossi/| 0939 | 0976 20 os68_| 0.664 og | 094 | 0977 30 os81_| 0.676 oes | 0943 | 0978 40 0.593 0.687 J 0x13 0.944 0.978 50 0,606 | _ 0.699 (_ ossX| os46 | 0979 60 oss | ovo | 0803/| osss_Kosas | 0980 70 oo31_| o7a | os | 0296 0.981 80 o6a3_| 0733 | ofa | 0903 | o95\] 0.982 90 0656 | 0744 | 6834 | 0911 | 0953 Nossa 100 0.668 0.756 __|/ 0.845 0.918 0.955 bas. vio | o6si1_| 0767 /|_‘osss | 0926 | 0957_ | “0.984 120 0.693 0. meh, 0.865 0.933 0.959 0.985, 130 0.706 0.790 0.876. 0.941 0.961 0.986 140 ons | odor | osss | 0943 | o92 | 086 si3_|_oas7 | 0956 | 0964 | 0987} 33Figure 1 Column System REFLUX VAPOR OVERHEAD STEAMIN LIQUID TO TROM PRODUCT TO REBOILER REBORER TANK ““TX* Numbers are the numbers of the input channels to the data acquisition system in order from top to bottom on the display. 34AKF H><- Wad L2Nd0Nd Figure 2 Reboiler, Pump and Tank System 35 eS 49000Nd “au,0 WwowdFigure 3 Heating SystemFigure 4 Glitsch Ballast Tray Details GLASS DISTILLATION “COLUMN GLITSCH BALLAST TRAY DETAILS 20". gp ee (HON Be = KARL- 140-06 31CALIBRATION CURVE REBOILER GLASS COLUMN T. Telford 7 Sep 198+ 38 5 a a § g z z E seyour ‘Hyaad 2e@rfr suet od peer ort yo +t ON = eet eo mt ee effete eee ee aFigure 6 T-x-y Diagram 1,1,1 Trichloroettane and Trichlorethene BF 30 UoRoE! OW gO SCO)... SO... 80 800. Oro. O80. O80 | OKO O00. i ae +0071 PAINS WO 81gqNG loos 4 jt @AIND JUIOg MEQ SS ee i ee ee | 00'98 o'Bap ‘eimeseduiay 39SUBYIEOO[YOUL |'E'} JoBy fou pnb] oF 60 80 £0 90 gO vo c0 xe) to nV PhO ZO €'0 70 3'0 Figure 7 40 90 xy Diagram 1,1,1 Trichloroethane and Trichlorethene -2'0 z 3 3 2 = F a 3 & g 8 > 8 3 80 60 ~O'b a ee a aaaFigure 8 Refractive Index 1,1,1 Trichloroethane and Trichlorethene oszet au ‘xepu] oAjowjoy, Sour’) Osey"k —ongp'L—Osse! —Oogh'L © osbert—obberL—asey't ore" 0 Ob 0 ee OL (au) ee'oes2 - zes'Zz/e = M] 08 aa el 001 3 ZOE 18 UONoBsjoY jo Xopul euejeoso] yop eUBYJeoIO[YoUsL 144) MA ‘ounypeouOYOHL EEL “Wd WM 41~40 -30 1.1509) 1400 1.1300. 0.300 Figure 9 Density of Ethylene Glycol in Water ; Degrees Centigrade -2% - 0 1 2 TUTTE ret | —JFREEZING GuAVE 95 Hi Jit 138 94 93 —je2 an L & | + | am 1 o mo % om mm ‘Temperature, Degrees Fahrenheit 42 vo Pounds Per Gallon/ Figure 10 ‘Viscosity of Ethylene Glycol in Water Degrees Centigrade <1 -2 -w 10 3. g 0 100% BY WEIGHT GLYCE i547 0 ” y 3 & 8 $ or 100 0 ° 0 109 Temperature, Degrees Fahrenheit 43