IFPTrainin Refining-Petrochemicals-Chemicals-Engineering DISTILLATION COLUMNS: OPERATION AND CONTROL ‘A~ ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC CONTROL SYSTEMS INTRODUCTION .....nnienncs Seti Seven |'- GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY... 2 Il. MATERIAL BALANCE FOR THE COLUMN 4 lll- OPERATING PRESSURE FOR A DISTILLATION COLUMN. 8 1 = Pressure profile 8 2 - Tray operation and pressure drop 9 3 - Pressure control, " 7 14 'V-_ ENERGY BALANCE AND LIQUID-VAPOR CIRCULATION INSIDE AN INDUSTRIAL DISTILLATION COLUMN nc... 1 - Energy balance for a disilation column - 14 2 ~ Condensing rateQo Be : 5 5 3° Function of the external refiux . . 16 4 = Reboiing rate OR eee 8 5 - Function ofthe vapor produced in the reboiler : 2 6 - Control of the reboller duty i 2 7 Molar fow rate profiles in a distilation column siaes V-_ TEMPERATURE AND CONCENTRATION PROFILES IN A DISTILLATION COLUMN.......34 1 = Concentration and temperature profiles in a column processing a binary mixture 31 2. ~ Concentration and temperature profies in a column processing a complex mixture with more than two components. ¥ 32 DT BIN -01312.A_A-Rev.3 ‘6102/2011 a 02itt ire trainingB - OPERATING VARIABLES IN DISTILLATION COLUMNS - CONTROL CONCEPT OF DISTILLATION COLUMN SEPARATING POWER ~ Number of theoretical separation stages. + Liquid-vapor circulation = Feed inlet location, a ~ Separating power to meet a given separation problem ~ Adapting separating power to separation difficulty Il VARIATIONS IN A DISTILLATION COLUMN'S SEPARATING POWER 1 ~ Increased reflux and reboling rate with a constant cut point. 2 ~ Influence of the new separating power on resulting separation, Ill VARIATION IN THE MATERIAL BALANCE FOR INDUSTRIAL COLUMNS - ‘SENSITIVE TRAY TEMPERATURE CONTROL ..0..cssesssnmnceennnn Impact of disturbances on distillation column operation + Change in the cut point by increased reboiing. ~ Changing the cut point by other types of action = Concept of sensitive tray : ~ Implementing sensitive tray temperature contro ~ Advantages and limits of sensitive tray temperature control IV- CHANGE IN FEED CHARACTERISTICS 4 = Change in feed flow rate 2 - Change in feed temperature... 3. = Change in feed composition V- CHANGE IN A DISTILLATION COLUMN'S OPERATING PRESSURE 1. + Modification in operating pressure - Increased pressure. 2 = Comparison of column operation at two different pressures ii 2 3 4 3° = Adapting the column to changes in operating pressure - implementing quality reguiators... O12 AA ©2011 - IFP Training we AB 43 43 45 46 48 50 60 57 57 61 63 68 69 wT 72 74 son 78 78 on T9 81oOINTRODUCTION ‘The purpose of most of the courses dealing with the distillation process as itis widely used in the chemical {and oil industries is to describe the engineering methods used to solve problems in designing columns so {fal they can meet specified separation requirements. Solving such design problems means choosing the operating pressure and determining the optimum values of the parameters that define the separating power of industria columns: — the number of trays or height of packing needed, ~ the required energy expenditure that govems the column's intemal liquid and vapor circulation, = the optimum location for feed inet. Then in the operational context, aistlation problems are examined witha different approach. Industrial columns are designed fo achieve a given separation that may change with production needs. They are subjected to numerous disturbances of diferent origins and are operated by a contro! system that prioritizes some parameters with respect to others. The purpose of this paper isto discuss the operational behavior of industrial columns. By this we mean to analyze the way they operate regarding different types of changes in operating condltions and to show the possibilities and limitations of the relevant control systems that are implemented. Consequenty, the folowing study comprises two main parts * The first part aims to clarity the signiicance of the isilaion column's operating ‘Parameters: feed, products, pressures, profes of temperature and composition, molar flow rates and energy expenditures, etc. It also includes the description of the basic control ‘systems that apply to the major variables used in operation. * The second part covers setting parameters and the behavior of columns with respect to liflerent variations in operating conditions. It winds up with the justiication, advantages and limitations ofthe various control systems used on industrial columns. oA © 2011 -IFP Training= A- ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC CONTROL SYSTEMS ee ee eee I+ GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY The basic diagram of an industrial distillation column is given below. Counterourent circulation of quid and vapor is achieved inside the column by the external reflux injected at the top and by the reboiler which ‘Generates the vapor stream required by the process. The feed is incorporated in this cireuation by delimiting rectifying and stripping zones located respecively above and below the feed inlet. The liquid-vapor contacts that allow the feed components to be separated according to theit volatility usually take place on trays, The reboller, and even the condenser inthe event that overhead vapors are not totaly condensed, Constitute extra separation stages. In normal operation inthe diagram below, condensation is tlal and consequently the overhead product or distillate that comprises the volatile components of the feed is obtained inthe liquid state after condensation 2nd proceeds through the reflux accumulator. The bottom product or residue that contains the nonvolatile or heavy components is drawn of in the liquid state atthe bottom of the column, (7S convenser 2 Vapor Rae a @) distlate - uc}-s CLL REFLUX m3 n) | DRUM @) I = aaa DISTILLATE me or overhead product , a Gr) @) REBOILER \ Cn) 4s @ Ww) 4 __|___L. Reboiing liad medium X } RESIDUE : () or bottom product : @), i aR) o1si2 Aa ©2011 -IFP Training DreozThe instrumentation and control equipment on the column is quite conventional it includes: ‘An overhead pressure controller (PC) that acts frst on the cooling abil by the cold fluid flow rate and then on a reflux drum degassing valve. ‘An external reflux flow rate controller (FC) and at the same time a reflux drum level controler (LC) that acts on the distilate flow rate ‘A reboiler fluid flow rate controller, since the residue draw-off is under the contol of the: liquid level at the bottom of the column. Flow rate recorders (FR) for the feed, products, reflux and reboiler fluid. ‘Temperature measurements with indicators or recorders (Tl or TR): reflux drum overhead column reoffying zone stripping zone bottom ofthe column feed at the column inlet hot fui atthe reboier inlet and outlet ~ Two analyzers (AR) used to measure the impurity content in each ofthe two products. The control devices equipping the column is relatively simple. Pressure is regulated in most distillation columns. Control of the external reflux flow rate and control ofthe heat input fo the reboiler through the hot fluid flow rate is a very common basic setup. As shown later on, this implies leaving the distillate and residue being leaving the column without any flow control. This is achieved by subordinating them to the liquid levels in the reflux drum and in the bottom ofthe column respectively. The body of data provided by instrumentation (temperatures, pressures, flow rates, analyses, etc.) is used to assess process operation, which is the subject ofthe study in the following sections. The study deals mainly with the points listed below: oA the material balance for the column the internal pressure profle and pressure control the energy balance and the duty of the condenser and the reboller the concentration and temperature profiles ©2011 - IFP TrainingFEED Overall material balance = + cut point Light key: the heaviest ofthe light components Separating power separation line > MATERIAL BALANCE FOR THE COLUMN Under stable operating conditions, the amounts of matter that go into the column and the amounts that come out are equal. This is true from an overall standpoint, but also for each component of the feed. If the molar (or mass) flow rates of feed, of distilate and of residue are called A, D and R, the following ‘equation should hold true | a=p+r — |overabalence Likewise if the partial flow rates of any component i are called Aj, D; and R;, the following holds true: vapor, | Partial balance for component i ‘Accordingly, separation involving a mixture of n components will yield n material balance equations that can be broken down into n-1 partial balances and one overall balance for example. In practice, the column's operating conditions determine the values of D and R, which in turn define what is called the feed cut point. This concept is ilustrated in the diagram below. The feed going into the column is represented by a rectangle, with the different components a, b, c, d, e, and f appearing inside it in order of decreasing volatility. The area of each one is proportional to its concentration in the feed. The distilate- residue separation performed by the column is represented by a theoretical horizontal line dividing the feed into two parts: the light or volatile components concentrated in the distillate and the heavy components in the residue ‘+ Non cistiouted components eet * Distributed components. bed Heavy key: the lightest of the heavy components oA © 2011 - IFP TrainingThe feed cut point is also expressed inthe form ofthe ratio DIA. Itis located near the borderline between the ‘wo components in the mixture that are the most difficult to separate because their volatility values are so close. In the example in the illustration, the cut point is located near the borderline between components c and d. Separating the two is the basic function of distillation. This is why the two components adjacent to the cut point are often called the key separation substances, with the definition: = the light or volatile key, (LK), here component ¢ + the heavy key, (HK), here d ‘The separation therefore depends on: = the difficulty of the separation, which can be characterized by the volatility interval between the two key components or relative volatility, ~ the separating power of the disillation process. ‘As a result, a feed separation line rests horizontally on the cut point on the preceding diagram and delimits equal areas on either side, This line represents the real composition of the distilate and of the residue and shows how the impurities are distributed in each of the two products. These two lines give a synthesis of the result of separation and is very useful in analyzing the changes in ‘operating situations. It also shows that ~ as is often the case ~ only some of the components are distributed, ie. present at the same time in the distillate and the residue. In the diagram, a, e, f, and g are not distributed in both of the products and b is present inthe residue, but in @ very small proportion. The two key ‘components ¢ and d are obviously found on both sides. ‘In many instances, these considerations are used to simply the partial material balances by writing Aj = D; for the lighter components and Aj = Rj for the heavier ones. If the composition of the feed is known and if the analyzers provide the concentration in distributed components (mainly the key components), a material balance table can then be set up for each one, Figures 1 and 2 on the following two pages show the material balance for an aromatic hydrocarbon separation column and for a debutanizer: — The aromatics separation column processes a mixture of benzene, toluene and xylenes. it is designed to separate the benzene at the top with @ good degree of purty. The key separation components are benzene and toluene. — The debutanizer processes @ mixture containing litle hydrogen and light hydrocarbons from C; to Cyy. It yields Cy gases at the top in the form of a vapor distilate and a liquid distillate in the reflux drum, with a.Cs, gasoline cut atthe bottom, The light key is rebutane hete (nC) and the heavy key is isopentane ((Cs). Or AA © 2011 -IFP Trainingvores 21095 1699. ponent Ez (wana (408's1) (ypu aye moi <>, ae (ure) amnssaig CO) (0) ammeroduay, (esi) i CI NTR ea (cove) g SNIZNASTANLA ow |8 sowie je @ je (e320) * 3N3ZN3a £ {o. — a0uejeg sjeveyey — NWN109 NOLLWaWd3S 3N3ZN3a —Figure 1 — ©2011 - IFP Training oAHydrogene (om) Methane (068) DEBUTANIZER — Material balance — —Figure 2— © 2011 -IFP TrainingIll- OPERATING PRESSURE FOR A DISTILLATION COLUMN 1. Oi AA PRESSURE PROFILE The operating pressure for a distilation column is determined by the conditions that arise after condensation in the condenser or in the reflux drum, Under design conditions, this reference pressure is the vapor pressure or bubble point pressure of the iquid distilate, It therefore depends mainly on the distillate's composition and temperature, EES *+ The composition ofthe liquid ofstitte is a result of the nature ofthe mixture that is being processed, the separation specications and the corresponding material balance that can be deduced. + The temperature in the reflux drum mainly depends on the temperature of the cooling |___ fluid that is used in the condenser. The required separation determines the composition of the liquid distilate and the temperature of the drum is approximately 30 to 50*C under design conditions in the common setup where water or air is used as a cooling fluid. The temperature of the drum can be lower when chilled water or refrigerants are is used. This is necessary when components are distled whose critical temperatures are lower than the ambient temperature. On the other hand, it can be higher ifthe vapor pressure ofthe dstlate at ambient temperature is lower than atmospheric pressure. Here the temperature of the drum is usually kept slightly higher than the normal boiling temperature to avoid to operate in vacuum. CONDENSER Pressure drop Pon) Pressure drop on ays @) Based on the reference pressure Ph, prevailing inthe refux drum, a pressure profile is created in the Column which corresponds to the pressure losses that occur because of the vapor stream flowing {rom the reboiler tothe condenser. The value of the pressure drop APe due to the condenser and the averhead line usually ranges from 200 to 500 mbars. ©2011 -IFP Trainingos AA TRAY OPERATION AND PRESSURE DROP The pressure drop due to the trays Pp is the sum of the pressure drops caused when the rising vapors move through each tray. The value can vary from 3 to 20 mbars (design conditions). The figure below illustrates the circulation of and contact between the two liquid and vapor phases on a one-way tray. The pressure drop is the result of: ‘+ Making the vapor gain speed in a restricted cross-sectional area in the active part of the tray (dry tray pressure drop). + The resistance exerted by the layer of liquid on the tray (pressure drop related to the ‘vapor passing through the liquid phase). In an industrial column with fixed geometry, the through-tray pressure drop is therefore variable according tothe flow rates of liquid and vapor circulating in the column. In particular, any inerement in the hydraulic load of the trays causes an increase in the rising velocity ofthe vapors and a thicker layer of liquid on the tray as well. These two effects have the same impact, i.e. to increase the through-tray pressure drop. _- Downcomer AP : pressure dropper tray hip : weir height ‘height of quid above the weir ‘hp quid pressure drop in U-tum py : vapour pressure drop ©2011 -IFP Training10 It should be noted that the differential pressure from one tray to another causes an additional hydraulic load in the downcomer. The total height of liquid H above the tray level therefore corresponds to the sum of the following heights: ~ weir height (30 to 70 mm determined by design) hy, = height of liquid above the weir: e which depends on the liquid flow rat, ~ height of liquid due to the restricted cross-section for the liquid when it enters the tray (liquid pressure drop in the U-turn) py. ~ height of quid due tothe vapor pressure drop hy For nominal operating conditions, the height H reckoned in clear liquid is located approximately at the halfway point between two trays. The between-tray spacing generally ranges from 40 to 70 om. This height H varies depending on operating conditions and may reach the level ofthe upper tray when liquid and vapor flow rates are high. This corresponds to the flooding threshold and is detrimental to the column's operating performance. At high vapor loads, its also due to carryover of droplets of liquid by the vapor stream. This occurs when the droplets have not had enough time to settle out between {wo trays and are recycled to the upper tray. Recyciing this additional liquid overloads the liquid stream ‘and contributes to loading of the tray (looding by vapor). ‘Another cause of flooding is the liquid flow rate when itis too high. The liquid can no longer flow or separate properly from the vapor phase and eventually fills the downcomer. The simplified diagrams below illustrate these two types of flooding. In actual fact, flooding is usually due to both excess liquid and excess vapor flow rates at the same time, orcosian Normal tray operation Carryover and flooding Flooding (excess vapour) (excess liquid) oA During normal operation under design conditions, a pressure drop of 3 mbars occurs with specially sized trays, 6 to 10 mbars are the most common values and values of over 15 mbars can be considered high. In the usual setup, with columns of 20 to 50 real trays, the pressure at the reboiler is therefore 0.1 to 0.5 bar higher than at the top of the column. This is @ very slight relative Variation for columns that operate under pressure, but may be significant in columns operating under vacuum conditions © 2011 - IFP TrainingOsAA 11 Additionally, itis important to point out that the design programs used to size or simulate industrial Columns are generally able to deal with the pressure variations caused by the trays. Since these programs work on the basis ofa theoretical number of trays, an overall efficiency value E is required for real trays. inthis way, each theoretical tray can be assigned the proper pressure drop by using the following equation: P real tray AP theoretcal tay = “PSRNSY PRESSURE CONTROL The operating pressure of a cistilation column directly influences the operating temperatures, the fiuid characteristics (the vapor volume flow rate in particular), and the heat exchange conditions at the ‘condenser and atthe reboler. Variations in pressure are therefore likely to disturbance the operation ofthe column and may become very troublesome when a temperature contro is implemented to run the column. Numerous disturbances may cause pressure variations, e.g. temperature and flow rate variations in the cooling fluid, condenser fouling, and modification in process conditions. As a result, a control system for the operating pressure is usually provided for. Since the pressure is variable in the column, a particular pressure is controlled, often the pressure at the top of the column, The pressure in the reflux drum, on a particular tray or at the bottom of the ‘column may also be used. ‘There are a large number of pressure control systems that can be classified into two major types ‘according to which control variable is used: = adjusting the condensation duty by acting on the flow rate of cold fluid or by varying the heat transfer area in the condensation sector (submerged condensers) ~ adjusting the reflux drum conditions by gassing: hot bypass, outside gas makeup, or by degassing a Acting on the condenser duty The duty of the condenser can be regulated by acting on the cooling fluid flow rate or on the heat transfer area. The diagrams below show the principle of these two systems. In the cooling fluid flow rate method, the pressure controller acts directly on an automatic valve for liquids of on the fans (angie of blades or speed) for air condensers. 8 ©2014 -IFP Training12 ‘When the heat transfer surface area method is used, the area is made to vary by submerging a selected number of tube arrays in the condensates. Here the condensers are said to be submerged Controling the condensate discharge allows the area requited for condensation to be adjusted opcoarsic bb Adjusting the reflux drum conditions In these systems, there is no action on the condenser ~ its efficiency is what itis because of the cold fluid flow rate, the temperatures and any degree of fouling. Depending on its performance, the required corrective action is taken downstream at the reflux drum: ~_ by lower pressure conditions (when the condenser is too efficient) a vapor makeup is ‘brought about by bypassing the condenser or gassing is implemented with outside gas ~ by higher pressure conditions, (when the condenser is not efficient enough) degassing is performed Condensation duty: = too much: hat bypass = not enough: degassing prcoasa0 The diagrams below show examples of types of systems that use gassing or degassing! ~ gassing by bypassing the condenser or degassing atthe reflux drum Ors AA ©2011 -IFP Trainingon AA 13 = gassing by outside gas makeup or degassing It should be noted that in both cases, when the condenser is too efficient, gassing offsets the inadequate vapor pressure of the drum liquid. The liquid is no longer at liquid-vapor equilibrium, tis said to be subcooled. Subcooling is variable depending on the operating temperature of the drum and can be a troublesome cause of perturbances in smooth operation via the reflux. ©2011 -IFP Training4 IV- ENERGY BALANCE AND LIQUID-VAPOR CIRCULATION INSIDE AN INDUSTRIAL DISTILLATION COLUMN 1- ENERGY BALANCE FOR A DISTILLATION COLUMN Given the following symbols: A.D,R molar or mass flow rates Hp. Mp. h molar or mass enthalpies of the feed, the quid distllate and the residue Qc duty ofthe condenser Qg duty ofthe reboier, the energy balance for a column inside the enclosed area shown in the diagram below can be writen as follows (in coherent unis and disregarding heat losses): Energy balance Inflow Outfow —_ po AtHa+Qg = Dehp+Rehr+ Qe pcossaa + Thermal energy input by the feed A . 7%, It depends mainly on the degree of vaporization of the feed. + Heat input by the heating fluid at the column reboiler Qp. + Heat flow rates carried off by the products at the top and atthe bottom, ie. D. hp end Rohg + Heat flow rates removed by the cooling medium at the condenser Qo, Osta ©2011 - IFP Training5 2- CONDENSING RATE Qc. Depending on the physical state ofthe distiate, two types of condensers can be distinguished: total or Partial. A total condenser implies a liquid distilate, while a partial condenser involves a vapor or mixed distillate Total condenser Partial condenser Liquid distillate Mixed cistillate Vapor distillate ‘The function of the condenser is therefore at least to condense the external reflux of the column in all instances. Total or partial condensation of the distilate may be added For a total condenser, the duty Qc is defined on the basis of material and energy balances in the condenser area opcatstn =V, i the molar flow rate of the overhead vapors with enthalpy H, Lg _ is the molar fow rate of the external reflux. Then Vy=lp+D (material balance) Vy Hy = (Lo D) hp # Qc, (energy balance) Qc = (Lg + D) . (Hy =p). OA (©2011 -IFP Training16 For a total condenser, Qe therefore appears as the condensation heat of th the distillate, It can be calculated from the flow rates Lo and D and the data required to access the enthalpies: distilate composition, temperatures at the top of the column and in the drum. In many columns Qc corresponds to @ quantity of waste energy since it is degraded at the ambient temperature of cooling fluids such as water or air. The reflux ratio, rf is defined to characterize the condenser duty and the liquid circulation initiated at the top of the column by the external reflux. I is the ratio between the external reflux flow rate and the distilate flow rate Reflux ratio y= By introducing ¢ into the expression of Qo, we get: Qc=D. lre* 1). (Hy -Pg) This equation shows the existing proportionality between Qc and r; for a given material balance, (0 = constant) 3- FUNCTION OF THE EXTERNAL REFLUX QTSSASOSSAMENAEH A, — overeat vapors The external refx enters the column OVERHEAD LINE a sy in the liquid state on the top tray, a nn fui Prior to this, the same amount had to a CONDENSER — flow out of the column in the vapor Condensation SI3t® with the overhead vapors. The ithe extemal quid reflux receives a heat rate on the tefux top tray in the column corresponding to the amount of heat required to vaporize it this phenomenon of extracting heat by vaporization is what gives the term REFLUX vaporizing reflux that is sometimes RUM Used to designale the external reflux, Distilate or overhead product ors AA ©2011 -IFP TrainingOAA 7 Heat is extracted at the expense of the rising vapors on the top tray, thereby causing them to condense partially. This gives rise to @ new liquid flow called the internal reflux. Vaporization and condensation then proceed on each tray. The heat that is taken in this way from the column by the external reflux is later given up to the cooling fiuid used in the condenser. In summary, the external reflux acts as a device to extract heat from the column and then transmit it to the cooling uid in the condenser. ©2011 -IFP Training18 4- REBOILING RATE Qg The reboiler serves to partially vaporize the liquid in the bottom of the column in order to initiate a Vapor current. |ndustnal columns may be equipped with different types of rebollers, some of which ate illustrated below, Vertical or horizontal thermosiphon reboiler Vapour separation reboiler Kettle type This reboiler partially vaporizes the liquid from the bottom of the column and separates the resulting liquid and vapor phases. The liquid from the bottom of the column circulates naturally toward the reboiler where it is partially vaporized, Fired heater The liquid is taken from the last bottom tray and goes through the reboler once. The liquid and ‘vapor phases are separated in the bottom of the | The liquid from the bottom of the column is column, | pumped into the pipes of the fired heater where itis partly vaporized ois ©2011 -IFP TrainingFlow rate L = 140 kmolin Flow rate R = 50 kmol/h ao Lee Residue ‘Vaporization rate 30% mal Heating fui net, + Hosting id cut 19 The limitation of admissible vaporization rates often means that a device to segregate liquids needs to be installed in the bottom of the column, A standard setup for thermosiphon reboile's is shown below. A reboiled liquid can be drawn off as a residue that is not mixed with the liquid coming from the last tray. AA simplified diagram with a reboiler considered as a theoretical tray is shown below. O1AA BPCOSeIA The reboiler is fed by L', molar flow rate of liquid coming from the last theoretical tray with an enthalpy ny The streams coming from the reboiler Vig (enthalpy Hp) and R are considered to be in liquid-vapor equilrium, The material and eneray balances can be witten: Ly=VorR Ly ht, + Qg=Vp.Hy +R. hy Qg= Vig. (Hg hY) +R. (y= h'y) ©2011 -IFP Training20 Physically speaking, the duty ofthe reboiler includes: — an initial component corresponding to the vaporization of V'y since the difference H'y- hy corresponds to a latent heat of vaporization = a second component for warming up the residue from the temperature of the last tray to that of the rebollr, It corresponds to a sensible heat (hg - n'y) for heating a liquid Generally speaking, the vaporization partis largely dominant and this allows the relation between Qg and Vp to be prioritized. However, in some cases a significant variation in temperature between the last tray in the column and the reboier ora high residue flow rate gives particular importance tothe residue heating component. In actual practice, this formula cannot be used but Qz can, however, be reckoned easily by totaling the heat input from the external hot fluid that is used for reboling, If its flow is M and its enthalpy expressed in coherent units is H at the reboler inlet and H, at the outlet, then’ | Qg=M. (H,=Hs) This is the duty of the reboiler calculated on the basis of the characteristics ofthe reboiling medium In order to characterize the duty of the reboiler and the vapor circulation in the column, we define the reboiling ratio tp as the ratio between Vg and R, Le. Reboiling ratio puree = By introducing rin the expression for Qg we get: ry -R.(H’g-h'y) #R. (hg hy) Bee J ‘At a given cut point (R = constant) this equation shows the proportional relationship that exists between the duty ofthe reboler Qz and the reboling ratio r, oa AA ©2011 -IFP Training2 5- FUNCTION OF THE VAPOR PRODUCED IN THE REBOILER Flow vapor Internal refux Vapor generated wee REBOILER at the reboiler ~ Reboilng fluid —_ partial vaporization Liquid of the Residue 3 bottom of the column or bottom product B The vapor flow generated at the reboiler enters the column in the gaseous state, but prior to this an equivalent amount of liquid is fed into the bottom of the column from the last tray. This vapor flow is therefore condensed on the bottom tray by giving up an amount of heat which is equal to the amount that was required to vaporize it This heat input causes partial vaporization of the liquid coming down from the next-to-last tray, thereby generating a new vapor flow. It will proceed toward the tray above where it will in turn be condensed by vaporizing part of the internal reflux. This process is repeated from tray to tray and explains how there is @ continuous vapor fow from the bottom to the top of the column, 6- CONTROL OF THE REBOILER DUTY The control systems for distillation column reboiling vary widely depending on the type of reboiler used and the nature of the reboiling medium. AA distinction can mainly be made between: + Reboilers that use steam or a gaseous fluid that condenses. Here the heat rate ‘transmitted tothe reboier is proportional to the vapor flow thatis fed into the reboiler. If ‘Ais the heat of condensation ofthe vapor and Mis ts fow, then: Og=M.A OAA ©2011 - IFP Training2 As a result, Qg and therefore V'y are regulated by the vapor flow rate. orco ser Condensates + Rebollers with hot liquid where the amount of heat that is transferred depends largely on the average temperature difference between the reboling fuid and the reboiled fui. As @ result, itis not proportional to the flow rate of hot liquid. Given the possible disturbances, e.g. variations in pressure or temperature in the hot liquid Circuit, iis often advantageous to implement a system to control the transmitted heat rate opcostee + Fired heaters where the amount of transferred heat can be regulated by the flow rate of the liquid that is fed into the furnace and by its temperature a the furnace outlet ors AA ©2011 - IFP Training23 7- MOLAR FLOW RATE PROFILES IN A DISTILLATION COLUMN a+ Theoretical profiles with constant molar flow rates ‘The standard theoretical profiles of the liquid and vapor molar flow rates in a distilation column are shown on the diagram below. (Qc = Condensation heat Ca ) of V4 = (Lo + D) D bo V4 # Overhead vapor Alla, Va) v u Vaporized flow rate Qk = Vaporization in reboiler ofVo heating of R & Ya ——g— Molar flow rate These theoretical profiles are based on the Lewis hypotheses which say that the molar flow rates of saturated liquid and vapor streams remain the same in dstiation columns, In view of the condensation and vaporization that occur on each tray, this assumes that the molar heat of vaporization remains constant whatever the composition may be. More simply stated, this means that on a tray the amount of heat released by the condensation of one mole of vapor is equal to the amount of heat required to vaporize one mole of quid. O11 AA ©2011 -IFP Training ppcpastcOSA 24 The Lewis hypotheses = constant molar heat of vaporization and condensation ~ each mole vaporized is replaced by a mole that is condensed; = the molar flow rates ofthe saturated liquid and vapor phases remain constant. Starting with the molar flow rate of the external reflux Lo, the flow rate of the internal reflux in the rectifying zone L is, however, a litle higher than Lo, This corresponds to an amount of condensed liquid L that is greater than the amount that was vaporized Lo, The external reflux is not in fact injected in the saturated liquid state but as a subcooied liquid. This is due to the fact that the pressure at the top ofthe column is higher than the reflux drum pressure. As a result, even ifthe external reflux is a saturated liquid in the drum, its in the subcooled liquid state at the top ofthe column, The consequence is additional condensation of vapors which corresponds to the heating required to bring the subcooled reflux back to saturation conditions. The vaporization and condensation process then proceeds on each tray, thereby maintaining the ‘continuity ofthe internal reflux all along the column. According to the preceding hypotheses, ths yields a constant internal reflux flow rate L in the rectifying zone. The contribution by the liquid part of the feed La gives rise to the constant internal reflux in the stripping zone L' The stream L’ obtained at the bottom of the column is fed into the reboiler and is partially vaporized. This generates the revaporization flow V'g that returns under the last tray in the column. ‘The nonvaporized part ofL’ makes up the residue of the bottom product R. Vo then gives rise to V' the molar vapor flow rate which remains constant throughout the stipping zone. When the vapor flow goes through the feed inlet tray, it incorporates the vapor part of the feed Va, \hich results in V, the molar vapor flow rate in the rectifying zone. The overhead vapor flow V, is. totally condensed then divided up into external reflux Lo and the overhead product or distillate D. © 2011 - FP Training25 b- Significance of rectifying and stripping zones The discontinuity of lquid-vapor circulation that appears at the feed inlet level defines two zones in the column: + The rectifying zone at the top, characterized by: L + aratioy <1, - adifflerence V -L which is constant at all levels and equal to the distlate flow rate, The stripping zone at the bottom where there is: Lu + aratio ip >1, + adifference L'- V' that is constant and equal tothe residue flow rate. The difference in the names is related to the treatment given to the prevailing stream in each zone: a ‘vapor is rectified and a liquid is stripped. + Validity of theoretical profiles - Real profiles In actual practice, the Lewis hypotheses are of course never bome out absolutely since the molar heat of vaporization usually varies with the composition. The hypotheses do, however, give a fairly good picture of reality in many cases. This is particularly true when the different components of the processed feed have neighboring volatity values and form a mixture that behaves like an ideal solution. The preceding condition usually assumes that the components belong to the same chemical family. When the volatity values are very different -- which yields quite a wide temperature gradient in the column -- considerable deviations can be seen from the Lewis hypotheses. By way of an example, Figures 3 and 4 on the following pages show the profiles of molar fow rates calculated in the aromatics ‘separation column which was discussed earlier. The hypotheses of constant molar flow rate are fairly well verifed. In contrast, the debutanizer is seen to have quite wide variations in fow rates. The simple model of the Lewis hypotheses does, however, provide @ simple way of assessing the variations in liquid and vapor circulation inside industrial columns, OA ©2011 -IFP TrainingSaTId0Ud 31VY MOTs YVIOW NINN109 NOLLWuvd3s 3N3Z38 —Figure 3— (©2041 -IFP Training On AAoo0e 007 oor S31I40Ud SALVY MOT4d YOdVA aindl waZINVENGaG fea="ovm/ ees — 8 —Figure 4 — ©2011 -IFP Training oni AAoA 28 d- Internal reflux The real profiles and even the theoretical ones show a flow rate discontinuity between Lg external reflux and L the intemal reflux. The discontinuity is because the external reflux is subcooled as ‘mentioned earlier and can be explained basically by two causes. +The pressure at the top of the column is greater than the pressure in the reflux drum, except in special cases. Even ifthe reflux is at its bubble point under drum conditions, the external reflux is subcooled at the higher pressure prevaling a the top ofthe column, + Some pressure control systems, e.g. submerged condensers, use of gassing, cause the reflux to be subcooled right from the reflux drum and this intensifies the first cause. Accordingly, variations in temperature at the reflux drum can cause changes in internal liquid circulation at a given extemal reflux flow rate. They can consequently be @ source of disturbances that {rouble smooth operation of the column. When this is the case, it may be advantageous to implement ‘an internal reflux flow rate control system. ‘Specialists in process control usually employ a simple equation to calculate the intemal reflux flow rate from physical parameters that are easy to measure. Leg (t +kat) | Literal refx fow rate Ly extemal refux flow rate At temperature af the top of the column - temperature ofthe drum k constant to be determined depending on process characteristics ‘An internal reflux flow rate control system is implemented according to a setup of the type shown below. ©2011 - FP Training29 It can be noted that when the temperature in the drum decreases, this system normally causes @ reduction in the external reflux flow rate in order to get a constant internal refux flow rate, In contrast, since the same behavior is foreseeable when the temperature atthe top of the column increases, i is easy to see that this control system can operate properly only when the temperature al the top of the ‘column is also regulated - Feed inlet The profiles show a discontinuity in the vicinity of the feed zone which is materialized in the context of the Lewis hypotheses by the equations below: { VEV EVA LeL+la In actual fact, the profile discontinuities comply with these equations quite well Accordingly, the two liquid and vapor streams are seen to increase when they pass by the feed inlet zone, except when the feed is at its bubble point, Fossa vev = L=LtA ane aan cor when it is atits dew point, Feadat ts dew pot ou ©2011 -IFP Training30 It is also necessary to consider the case of feed introduced as a subcooled liquid or as a Superheated vapor in some particular columns, For both, induced streams are generated when the feed comes back to equilibrium conditions, * Vapor condensation and generation of an additional induced reflux when the feed is subcooled. ver Suteooed A aN | | . — 4 LoL+a Licuid feed rept { VeVi +A seta Superheated A vapor feed — onosnor The same as for the external reflux-internal refux relationship, the induced reflux flow rate can be calculated by the energy balance. Osa © 2011 - IFP Training31 TEMPERATURE AND CONCENTRATION PROFILES IN A DISTILLATION COLUMN 'As soon as the operating pressure has been determined, the temperature profile in a distitation column will match the variations in circulating stream composition more or less explicitly. The temperatures that become established are in fact equilibrium temperatures that correspond to saturated products: vapors at their dew point and liquids at their bubble point. At a specified pressure, the ‘temperature that prevails at a given point in the column characterizes the overall composition of the mixture inside the column, ‘At a given pressure, the variation in temperatures is therefore directly related to the variation in liquid and vapor stream concentrations on the trays. The temperature-concentration relationship is simple to assess for binary mixtures, It is litle more complicated for complex mixtures and may eventually involve éraw-ofs. The temperature at any point ina column is related to: = the composition ofthe vapor at this point (dew-point temperature ofthe vapor), = the composition ofthe liquid at this point (bubble-point temperature ofthe liquid), = the operating pressure. 1- CONCENTRATION AND TEMPERATURE PROFILES IN A COLUMN PROCESSING ABINARY MIXTURE It is easy to interpret the variation in component concentrations in the streams circulating inside a distilation column that processes a binary mixture, since there is only one volatile component and one heavy one. I we focus on the mole fraction of the volatile component (a) in the liquid phase, we can see that it will reach a high value close to 1 in the distillate and in the reflux Lg; it wll have a value close to zero in the residue (provided of course that the aim is to separate the two components proper'y). The mole fraction of the heavy component (b) is the complement of 1 cited for the other fraction and therefore varies symmetrically in the opposite direction, If the pressure is assumed to be constant, the corresponding temperatures are given by the isobaric liquid (or vapor) composition-temperature equilibrium diagram, t t (°C) ® At (°C) | | a ‘Mole fraction in A on AA ©2011 -IFP Training Bottom temperature Overhead temperature prmowe32 When good quality separation is sought, numerous trays will work at each end on a very small concentration interval. As such, the profiles have an asymptotic shape as shown in the diagrams below. —. Liquid phase temperaure 0 1 ‘mole fraction temperature a ‘An examination of the profiles raises the question of the best position for introducing the feed into the column. So that the variations in composition are not thrown off, the feed is introduced in such a way that its liquid fraction composition is close to that ofthe internal reflux with which it is mixed. For binary mixtures, this means seeking identical temperatures. 2- CONCENTRATION AND TEMPERATURE PROFILES IN A COLUMN PROCESSING ACOMPLEX MIXTURE (MORE THAN TWO COMPONENTS) The variations in composition in @ column processing a complex mixture are much more complicated In a simple practical approach, one can look a the problem from the standpoint of total reflux. This special case will be used to show the phenomena that are preserved as demonstrated by simulation studies under normal operating conditions 4 Study of concentration profiles in a column operating with total reflux Total reflux operation is ilustrated by the figure below. O1SIAA ©2011 -IFP TrainingOrsi AA 33 This is @ column where a given amount of feed A has been introduced. The feed circulates around repeatedly and holds the cut point at the required value via the system of retention at the top and bottom of the column. if tray holdup is disregarded, the amounts retained in the reflux drum and in the reboiler are D and R This type of operation is governed by relatively simple laws. A material balance set up between any two theoretical trays p and p + 1 including the top ofthe column gives: Vps1=ly pet Vp + 1>Lp are the overall molar flow rates that circulate between the two trays. Likewise, ifthe mole fractions of i in Ly and Vp, ; are called Xp and Yip . 1, @ partial balance on component i cives: or: Yip +4 = Xip (1) This relationship shows that with total reflux the streams that meet between two trays have the same composition. Additionally, the thermodynamic equilibrium at tray p + 1 involves the streams that leave the tray, Vp +1 and L, « 1. The corresponding compositions yp . ; and Xip . are therefore related by the equilbrium equation: Yip 1* Kip + 1¥ip+ t when Kip + is the K value of component ion tray p + 1 p+ yp ©2011 - FP TrainingOrs AA 4 Given equation (1), this leads to Xip = Kip +1 %ip +4 ‘As such, two consecutive mole fractions of component iin the liquid phase are related by the K value ‘of the same component i on the intermediate tray. | IFK}> 1 (light) x increases when rising IK; < 1 (heavy) x; increases when coming down So itis of interest to examine the variation in the value of the K factors all along the column. Very approximately, it can be estimated by using the simplest form of the K value taken from Reoul’s law (liquid: ideal solution, vapor: mixture of ideal gases). If the vapor pressure of component i at a temperature t and a pressure P is called PS), then: In the column: = the total pressure P can be considered constant in an simplified approach, - the vapor pressure of component i, PS, decreases when the temperature drops, and this causes a general decrease in all the K; ror the bottom tothe top ofthe column, It can also be noted that Kj is equal fo 1 when ps = P, i.e. when the temperature t is equal to the boiling point temperature of component (pp) at the pressure P. ‘Asa result, for this component i at any pointwhere tf > typ, Kj>4, therefore this component will behave as a light component at anypointwhere —t¥ ¢ t § VAT ? ee tbpy tpg tpg — tpg, tbPyy tbe tbpg ; — — e— Light components Intermediate components — Heavy components From the standpoint ofthe value ofthe K factors, we can conclude that + Light components have a Kj that is always greater than 1, and therefore their ‘concentration inthe liquid phase increases constantly from bottom to top in the column (p> %ip + 4). + Heavy components in contrast decrease in concentration in the liquid phase from bottom to top in the column (Xp < xip » 1) + Intermediate components behave in two cltferent ways: = E> typ, then Kj> 1 and xiy >Xip 4 + ift< typi then Kj <1 and ip ‘S311d0Ud SuNLWaadWaL 1 NOLWavdas IN3ZNIE Og, St —Opt_—OEF= OZ} @0 —Figure 7 — © 2011 -IFP Training Os AAon AA 4 The influence of the heavy components in the feed on temperature variations can be noted in the diagram below. Backward shift of heavy components Decrease in the internal + — Volatility due to the feed Sharp decrease in volatility J at the reboiler \2 Dew temperature Bubble temperature of dstilate ofthe residue Pcoawac d- Example: Sidedraws ‘The maximum concentration values for some intermediate components in a distilation column mean that itis possible to use sidedraws to get a product with a high concentration in a given intermediate ‘component. The following separation can be performed for a mixture of three components A, B, and C whose Volatility decreases from A to C, assuming thatthe voiatlity of B is closer to A than to C. +— —Sidedraw sii |» fichinB = ——», ea 0 05 1 Concentrations in liquid phase ° co 188 ©2011 - IFP TrainingO1IAA 42 Here, the major impurity in the product that is drawn off is component A which can be eliminated by stripping ina further column, In fact, this use of sidedraws is almost common practice for another problem: separating the most volatile component from a mixture, such as for the benzene column. Because of processing or storage prior to distillation, the feed often contains small amounts of impurities that are more volatile than the target component. Impurities are often inert gases, hydrogen and others which cause a maximum concentration value to appear for the target component near the top of the column. This is what justfies recovering the product by sidedraw. The zone located between the sidedraw and the top of the Column, which is designed to eliminate volatile impurtes from the sidedraw, is sometimes called the “pasteurization” zone. Volatile impurities Voiatie impurities +ABCD 0 1 “TL. Molar fraction in liquid phase reo ren This layout is very common in petrochemical plant separations, In most cases, sidedraws consist in removing part of the internal reflux from the column. However, it should be pointed out that there are vapor stream sidedraws. This is true particularly in certain extractive dstilation setups where an intermediate component can nat be drawn off inthe liquid phase, since this phase is diluted by the solvent. On the other hand, the solvent's very low volatlty means that itis practically absent from the gaseous phase where a high intermediate component concentration ccan be found, thereby justifying a sidedraw. © 2011 -IFP TrainingoO