Chapter 9 Distillation 1 [1. FLASH DISTILLATION(闪蒸)] 2.CONTINUOUS DISTILLATION WITH REFLUX回流(蒸馏) [Action on an ideal plate] [Combination rectification and stripping (Fig.9.4-3)] [Trap: 疏水器; accumulator: 集液器; condensate: 冷凝液; fractionating: 精馏; reboiler: 再沸器] 2 a x FF x x F Condenser a F L n n L ya a Va n VLa xn qc Va x F n n n Ln x L a out y Heat a n a Control n y xan xn Vn 1Accumulator D y V L a L a n surface 1 Ln xa qc LVLanVnn y xnn Lxann 1n 1 n 1 y La xD a Overhead Reflux xnn x xnyLn nm D q 1 c VnL1n xVyannn11 product V b x L a m a a VnL1n x V xD n n 1 Lm D y nxn1 qm F yb Vb yc nLL1mn Vb q Feed q x y nxn1 cy Vn 1 c a x n 1 L mVn 1 Dmmxxmn m L x F xm D y yb b FV y b D n 1 V D m q b1 [Fig.9.4-4(p.104)] xmVVmV c m Lmynn11 xL 1 Lb x F VaLmy n 1 x DLmymVn 1 y xbV Lb xD xmm VxDmmmyLm1nyb11m b1 D b xb Va y xaVmm yxmmymmb1LVb1qry xb Reboiler 1 b x bD Vmmm mLm 1 Control x1m B V L Heat in q r qr V m 1 m m 1 surface y 2 a Lay x L x m 1 y LV b by L m m1 m m1 a m 1 m 1 b b m 1m B my1 m 1 mb r b b yx x B Bottoms product y La x mV 1 m xx1 q L x B 3 1)Material Balances in Plate Columns (1) Overall and more volatile material balances for twocomponent systems F DB (21(9.4-1) .3) FxF DxD BxB (9.4-2) Units D, B: kmol/h, F 、Dof 、F, W单位: km ol/ h F , xF kg/h, lb/h D xF、xD、xW:m ol分率 F , xF D xD xD , xF, xB: molar fraction, or mass xD W , xW fraction, dimensionless W , xL W L L FF,,xxFF DD xxDD W,,xxWW W F ,LL xF D LL x DVV B ,VV xB L 114 Eliminating B from eq.(9.4-1) and (9.4-2) gives D xF xB F xD xB D xF xB x x B Eliminating F xDDDgives xB F F xD xB B xD xF F xD xB (21.5) (21.5) (21.6) (21.6) 5 (2)Net flow rates •Net flow rate in the upper section /rectifying section D Va La (21.7) D Vn1 Ln (21.8) DxD Va ya La xa Vn1 yn1 Ln xn (21.9) •Quantity D is the net flow rate of material, DxD is the net flow rate of component A, all upward in the upper/rectifying section of the column. Regardless of changes in V and L, and x, y, the differences are constant and equal to D, and DxD, respectively. 6 •Net flow rate in the lower/stripping section B Lb Vb Lm Vm1 (21.10) BxB Lb xb Vb yb Lm xm Vm1 ym1 (21.11) •The net flow rates are also constant but are in a downward direction. The net flow rate of total material equals B; that of component A is BxB. 7 (3) Operating lines •Two sections two operating lines •Operating line for rectifying section Ln Va ya La xa yn1 xn Vn1 Vn1 (9.4-10) Ln DxD yn1 xn Vn1 Vn1 (9.4-11) Ln DxD yn1 xn Ln D Ln D (9.4-12) Slope of operating line in rectifying section less than 1.0 8 •Operating line for stripping section Vm1 ym1 Lm xm BxB (9.4-13) Lm BxB ym1 xm Vm1 Vm1 (9.4-14) Lm BxB ym1 xm Lm B Lm B (9.4-15) Slope of operating line in stripping section greater than 1.0 9 2)Number of Ideal Plates;McCabe-Thiele Method •McCabe-Thiele step-by-step construction for computing number of ideal plates(逐板计算法): Using equilibrium curve and operating lines. (1)Constant molal overflow恒摩尔溢流 Conditions: (1)nearly equal molar heats of vaporization of every component, (2)Sensible heats and heat losses omitted. (显热) (热损失) the molar flow rates of vapor and liquid are nearly constant in each section of the column, and operating lines are almost straight. 10 L LL V VL V V V F , xF D xD W , xW L LL VL FF,,xxFF DD VVL L L 11VL xxDD 1VL L 1 22V W , x W , x L WW 2 L 21VV V L 3 VL L L L 3 3 31V2V L 1 L VL 11 L L L 1 F , x 1312V L1VV 22 V L F 223 VV D 21L312 VL1V2 进料板 V V V V 1 进料板 x 32 进料板 D 1 V 2 3 V 进料板 3 2 L 1 B ,11x 12 132 B 1 V 1 3 1 进料板 11 Constant molal overflow of vapor(恒摩尔气流) V1 V2 Vn V Const(rectifying) V V V V Const ( stripping ) 1 2 m V1 V2 Vn V 常数(精馏段) L L L L 常数(精馏段) 1 2 n V1 V2 molal Voverflow Constant of liquid (恒摩尔液流) n V 常数(提馏段) L L L L 常数(提馏段) 1 2 n L L L L const (rectifying) 1 2 n L1 L2 Lm L const( stripping) Units of above parameters: kmol/h 12 Operating lines becomes L Dx D xn Rectifying section yn 1 LD LD Stripping section L BxB ym1 xm L B L B 13 (2)Reflux ratio: RD or RV L V D RD D D and L L RV V LD (21.18) In this text only RD will be used. L Dx D yn 1 xn LD LD RD xD yn1 xn RD 1 RD 1 (9.4-18) 14 RD xD yn1 xn RD 1 RD 1 Construction of operating line of rectifying section:When When xD()xD , xD ) When xn xDx,n yn x1 D, xyDn 1 (xxDD , xD /( RDx: D/( 1)RD 1) y intercept (截距) 15 When xn xD , yn1 xD ( xD , xD ) xD /( RD 1) operating line of rectifying section When xn xD , yn1 xD ( xD , xD ) xD /( RD 1) When xn xD , yn1 xD ( xD /( RD 1) 16 yy11 V1 y1 V1 (3)Condenser plate LL and top D y1 L y1 V1 xx1 Partial xD x V1 1 LTotal condenserL 1 condenser y1VVV V V 1 1x V Vapor 1 Vapor xVapor V V 1 y1 C xD x1 1 11 L yyy 2 y1 y1 y V1 1 2 y y1 V yV1 2 V1 L 1 L L y1 x1 LLLCC DL D L Liquid LyLiquid C y1 x1 y2 2 V xxxC x x L 1 1 x 1 x C L x x x D D 1 L V LC D1 1 C C y 2V Final V V y D x1 x x VxC 1 xCV xxDC y1C xcondenser x1 y2 D D Liquid y2 y2 VPlate1LCy 2 x y y y y 2 V xC x2D y1D D LC 2 LC (b) LC (c) y 2 xCLC x x y (a) x C D 1 L L C y2 D xC y C C xC xC LC x y C xC xD y1 x x C LC C C 17 xC y x x1x1 y xD •When a total is used, triangle xxDD condenser x1 Vplate 1 abc in Fig.9.4-6a represents the top in the xxCC xD y1 column. (三角形) aa y1 x D y xD x1 xD xC a b xC bb a y1 x D cc b aya1 xyDc x D byb xxD1 a cxc1 x Db x D xC c (a) xC a a b L Total condenser V1 Vapor V V1 x1 y1 y1 V L DL y 2 D Liqu x1Liquid x xDx1 LC D D Final V x x y1 xCV xxDC y1C xcondenser D D y2 y xC xD yy 2 LC (b) LC y 18 xC x xD y y1 x D D xused? 1 •Question: Why is the partial condenser xCx x1 y xD C x D •For a partial condenser,xC is in equilibrium with y’, a V1 xD a x1 or xD. The partial condenser, representedxCby the b bis equivalent y1 xC dottedV1triangle a’b’c’ in Fig.9.4-6b, x D to a a theoretical y1 cxcD a y1 L plate.D[分凝器相当于一块理论板] xC b Partial xD x y axaD byc1 x Da L 1 condenser V1 V b x y x V1x1 Vapor xVapor y x bD cya x Db C D 1 11 y1 y c y yV1 2 x y D yxcD xaxb1 c 1 D L L LyLiquid C xx1C y xbxcD 2 a D x1 x x xL xaD x cCy1 xbD 1 C C 1 Final V D y x a x V D b C xC x Liquid condenser c D y2 x (b) 19 D D x b y2 1 c a x Dx y1y x Dx 1 D y1 xC y y xDx y1D x D •(y1, xC)Vis on operating RDx1x1 yy1 xxDxDD 1 y1 x line of rectifying section. x Dx Cy x D RD 1D x1 RD y1 1 xD(y , x )的交点在操作线上。 V1 y1 1 C xCx x1 V1 y1 LC CxC xD DxDy xD D y1 L a a xD x1 xC Partial LC b x xD x L 1 b aC RD xD condenser V c yD x a Vapor cD b V xVapor 1 V11x1 Vapor xC C x D y1 y axaD byc1 x Da y1 y y V y 2 1 yx11 bxbD cya x Db L L LyLiquid C 2 1 yxD cyxcD xaxLiquid c bD x 1 1 x L x C xx1C y xbxcD C 1 a D V Final D y x x c 1 D a C xD x x VC b Liquid condenser 1 y x a y2 D xD D xbC x c y D 2 x b ( b ) 1 c 20 a x L C LC xC x xD y1 y xD x Dx y x D xxDD y y RD y1 xD x D y1 D x1 y1 xx xC x x Cx 1 1 1x RD 1 R 1 y D x D y C D a a xD •When condenser is used, triangle DD V1ay1partial xxL x Dx x1 D x1 C C xC a’b’c’ in Fig.9.4-6b represents the top plate in b x x x LC CC b aC x xD D R the column. D cxcD a y Daa 1 xC xC b axaD by1 x D b b y y1 x D a a c b y xD y x c c c x y x b 1 D 1 1 D b b a y xD c x1 aya1 xyDc x D a x c y x D c x1 y1D xbD x byb xxD1 a b x D x a 1C y x c xD D x x cc1 cCy1 xbD x Db a x D x xC 1 y x x D xC a D b x c c C a xD 21 xC a bx1 c y1 xC 1 •When condensate is liquid at its bubble point, L=LC, V=V1. •If the refluxVV is11 cooled below the bubble point, a portion V1 yy11 of the vapor coming to plate 1 must condense to heat V1 y1 V1 the reflux; soLL V1<V and yL>LC. D y L V1 xx1 V1 1 V y1V V V 1 y1 1 L yyy 2 V1 V1 L 11 2 x1 LLLC y1 y1 x1 C V xxxC L L V 11 C y 2V x1 x1 y2 VPlate1LCy 2 V LC 2 xCL y 2 (a) y xC CC 2 L xCC LCC xC 1 1 Partial xD x L LTotal condenser 1 condenser V1 Vapor V1 V Vapor V1 x1 V1x1 Vapor x C xD y y1 y1 y y y1 V yV1 2 L L D DL L Liquid LyLiquid C y2 2 x x1 x x Dx11 LC x D D xL C 1 C Final V V y D x x V VxC 1 xC xxDC y1C xcondenser D D Liquid y2 y2 x y y y 2 xC yx2D y1D D LC L xC x Dx D y1 (c) LC (b) y LCC xC xC y x x y x x C C C D 22 1 •the reflux is cooled below the bubble point, so V1<V and L>LC. L cT (TT TC ) L c ) C( pc 1C L c ( T T ) C pc 1 L T C pc 11 T CC ) L (21 21 .21) Cc pc ( L L L (((21 L c ( T T C LL L LLC L L 21 C) L C pc 1 21...21 21))) CC C L LCCC L (21.21) CC c LCheat c pc (T condensate TC ) ccpc c 1 =specific of pc pc L cLpc (21.21) pc C L T of TT111 =temperature C liquid on top plate T1 T1 c pc TTCC TCC =temperature TC of returned condensate CC of vaporization of condensate CC = Cheat [1 c pc ((TT11 TTCC ))cc ]] C TC R LL LLCCC LL LL CC [1 cpc pc (T1 TC )c ] ((21 ..22 )) L [ 1 c L L L D C pc 1 C c R 21 22 C DD D c column cthen ] (21.22) D RD actual D L reflux LC ratio L LinC [1the pc (T1 TC )is D D D •The C RDD D (21.2 D )c ] L LCD L DLC [1 c pc (T1 TCD RD (21.22) D D D T1 23 (4)Bottom plate and reboiler •For constant molar overflow L BxB ym1 xm L B L B (9.4-21) •Construction of operating line of stripping section •When xm xB , ym1 xB ( xB , xB ) L L slope L B V 24 ui cu libr r v iu e m Op era lin ting e x= y Eq yb yy b b a yb r yr d y c yr x b y B xxbB y b y r x B e x b xb 1 y r x B xb xb 1 x x xb 1 B b xbx xb 1 x 提馏段操作线过点(xB,xB) •Construction of operating line of stripping section •When xm xB , ym1 xB ( xB , xB ) L L slope L B V 25 xb x Plate b by b V yr b b L xb V V yr yr B B a xB y x Bb r yr x y B xx B L xb Op era lin ting x= e y yb yy b B xB Eq ui cu libr rv iu e m V L L yr xb xb B V Column V xB sump yr yr B 塔底集液层 B xB xB d yb y bc y r yr xB e xxbb1 y r x B x b 1 x x B b x xb x b 1 L L xb xb V V yr yr B B xB xB Steam Condensate •The vapor leaving the reboiler(yr) is in equilibrium with the liquid leaving as bottom product( xB ). The reboiler acts as an ideal plate再沸器相当于一块 理论板. 26 (5)Feed plate •At the plate where the feed is admitted, the liquid rate or the vapor rate or both may change, depending on the thermal condition of the feed(进料热状态). •Five different feed types: (a) feed cold liquid 冷液进料; (b) feed saturated liquid饱和液体 进料; (c) feed partially vaporized汽液混合物 进料; (d) feed saturated vapor饱和蒸汽进料; (e) feed superheated vapor过热蒸汽进料. 27 •Thermal condition of feed进料热状况. •Material balance about feed plate F V L V L •Enthalpy feed FH Fbalance V H V ofLH L VH V L H L Fplate V L FVVL L V L H H ,H H V L FH V H LH LVH V L H L FH F V H V LH F LH V L VH V L HV H F L L , HL HL H V H V , HHLV HHLV HV H L F H V H F HLV LH F L L Hence H V HF L L VF H L F HV H L q H HV H L F H V H F HLV LH F L L q qDefine F H V H L H VF H L V L 28 HV H L F HV H F L L Define q HV H L F q = parameter of thermal condition of feed进料热 状况参数, or moles of liquid to stripping section of column per mole of feed进料液化率 For cold-liquid feed H V c pLTb H F c pLTF H L c pLTb c pL (Tb TF ) q (9.4-22) 29 H L c pLTb c pL (Tb TF ) For cold-liquid feed q c pL , c pV = specific heats of liquid and vapor, c T c pLc ,pLc,respectively pV pV F cF pL=, cFtemperature V L V L of feed pV Tb ,TTFT d F V L V L T FH F V HV point LH L VH V and L H L dew point b ,F TbT,TT of d =d bubble FH F V HV LH L VH V L H L HV , H L H L TdHV respectively Tb ,feed, (泡点) (露点) HV HV , H L H L HV H Fof vaporization L L = heat H H L L HV H L vapor F •For partially feed, 0<q<1 HV H L F L L q L L qF L L qF F V F 30 HV H L F HV H F L L HDefine qd V c pV T HV H L F H F c pV TF For superheated vapor feed H L c pV Td q c pV (TF Td ) (9.4-23) 31 F V L V L FH F V HV LH L VH V L H L HV HV , H L H L •Material balance of feed plate HV H F L L F V L HVV HL L F FH F V HLV L LH qF L VH V L H L HV HV , H L H L V V (q 1) F (9.4-25) H H L L V F H LH VH L H FH V V FV (1V q) F L V L HV H L F LH H FH HVVH, H VH Visvaporized进料 LHL L (1 q ) H f V =Ffraction of feed LL that V HV H F L L HLH L L , H H FH F VqH HVVV汽化率 VH LHL F L V L L V HV H L F H, VH H H 32 H HH LH L F L V V V L F L V L V L F L F F L L L V V L V (a) V F L V (b) V L V L L V (c) V F L L V V (d) L V L V (e) 33 HV H L q Values of five feed types V L F F HV H F L L q HV H L F V L F L F L V L (a) V Cold feed L H F H L ,F q 1 (b) (c L V V F V V,L L F 34 HV H L q Values of five feed types V L F HV H F L L q HV H L F V L F V L F L L (a) V V (b) (c) L V point (saturated liquid V Feed at bubble L F H F H L , q F 1 ) 饱和液体 V V,L L F 35 HV H L q Values of five feed types V L V L F HV H F L L q HV H L F F L L (b) V V (c) L F Feed V partially vapor HV H F H L , 0 q 1 V V,L L L F 36 HV H L (a) of five feed types q Values HV H F L L q (b) HV H L F L V L F F V F L L V V (d) (e) Feed at dew point (saturated vapor) HV H F , q 0 V V F, L L 37 ( (d) HV H L F HV H F L L q Values of five feed types q HV H L F (b) (c) L V V F L L V (e) V Feed superheated vapor HV H F , q 0 V V F, L L 38 Question: Bubble point feeds, given F1F,1F, 2F,2V,V, L, L isisgiven ,, F1 , F2 ,V , L is given, F1 , F2q,V , , q L , V is , L given is given , , L ?V,?,VL, Lis is VV1 F ?2 ?LF , F , F , given given , , V ? L ? F , F V , L is given , 1 1 2 2 1??L 21 2? V ? L V F1 , F2 ,V q1,,VLqV2 , V?, ,given L is ,given , is ?, L ? L ? V V ? L ? L ? ? V ?, L ? V ? L ? V ?, L ? V ?, L ? V ?V L?? L ? ?, ?, L? ? ? V L?, L VV ?, ? V F, ?, L ? V L 1 F2 , V , L is given, V V V L L F1 L L F2 L F1 F2 39 (6)Feed line •Feed line进料线 ----Line of intersections(交点) of the two operating lines. Equilibrium line d Operating line of rectifying section Operating line of stripping section xB xB xD 40 •For constant molal overflow(恒摩尔流), the operating line equations for two sections are L Dx D xn Rectifying section yn 1 LD LD Stripping section L BxB ym1 xm L B L B 41 That is Vy n1 Lxn DxD (9.4-26) F xVm LBx V B L V ym1 L (9.4-27) FH F V HVthe LHoperating L VH V L H Llines To locate the point where HV =y, HV , HxnL =x HmL =x and intersect, let yn+1=ym+1 subtract Eq.(9.4-27) from : HV H Eq.(9.4-26) L L F y(V V ) ( L HVL )HxL Dx F D BxB FxF DxD BxB L L qF V V (1 q) F q xFFH F V H V LH L VH V L H L y x (21.31) 1 q 1 HqV H V , H L H L 42 q xF y x (21.31) 1 q 1 q •Eq.(21.31)represents a straight line, called the feed line, on which all intersections of the operating lines must fall. •The position of the line depends only on xF and q. 43 (7) Construction of operating lines •The simplest method of plotting the operating lines is to q 1 (1)locate the feed line: q xF y x 1 q 1 q (21.31) When x xF , y xF ( xF , xF ) 0 q 1 q 1 q0 r q0 q slope 1 q xF 44 (2) Construction of operating line of rectifying section:When When xD()xD , xD ) When xn xDx,n yn x1 D, xyDn 1 (xxDD , xD /( RDxD/( 1)RD 1) y intercept: When xn xD , yn 1 xD ( xD , xD ) xD /( RD 1) When xn xD , yn 1 xD ( xD , xD xD /( RD 1) operating line of ) rectifying section When xn xD , yn 1 xD ( 45 xD /( RD 1) (3) Draw the stripping line through point (xB,xB) and the intersection of the rectifying line with the feed line. 0 q 1 xB xF r xD xB xD RD 1 xB xB xF xF xD xF 46 (8) [Optimum] Feed plate location(适宜的进料位置) When should the steps transfer from the rectifying line to the stripping line? The change should be made in such a manner that the maximum enrichment per plate is obtained, so that the number of plates is as small as possible. The transfer should be made immediately after a value of x is reached that is less than the x coordinate(坐标) of the intersection of the two operating lines. 47 Optimum feed plate location: plate 3 a Feed plate 3 b 5 How many ideal plates are needed? r Reboiler? Partial condenser? xB xF Optimum feed plate location? xD Is the number of ideal plates related with feed flow rate F? 48 Problem A continuous rectifying column treats a mixture consisting of 40% weight benzene and 60wt% toluene at the rate of 4 kg/s, and separates it into a product 97 % benzene on the top of column and a liquid containing 98wt% toluene at the bottom of column. The feed is liquid at boiling point. (a) Calculate the weights of distillate and waste liquor per unit time. (b) If a reflux ratio of 3.5 is employed, how many plates are required in the rectifying part of the column ? (c) What is the actual number of plates if the plate efficiency is 60%? 49 Mol 0.1 0.2 0.3 Mol fraction of benzene in liquid: 0.4 0.5 0.6 0.7 0.8 0.9 fraction of benzene in vapour : 0.22 0.38 0.51 0.63 0.7 0.78 0.85 0.91 0.96 50 Solution The equilibrium, data are plotted on Fig. llh. As the compositions are given as weight %, they must first be converted to mol fractions before the McCabe-Thiele method can be used. Mol fraction benzene in feed (40 / 78) 0.44 x f (40 / 78) (60 / 92) Similarly, xd=0.974 and xw=0.024 51 •[EXAMPLE 21.2(a)(b)] 52 •As the feed is a liquid at its boiling-point, the q-line is vertical and may be drawn at xf =0.44. (a) A mass balance over the column and on the more volatile component gives in terms of mass flow rates: • 4.0 = W' + D' 4× 0-4= 0.02W' + 0.97D' from which: W' gives = bottoms flow rate = 2.4 kg/s And: D'=top product rate = 1.6 kg/s ' 53 (b) If R= 3.5, the intercept of the top operating line on the y-axis is given by xd /(R+1) = 0.974/4.5 = 0.216, and thus the operating lines may be drawn as shown in Fig.11h. The plates are stepped off as indicated and 10 theoretical plates are required. (b) If the efficiency is 60%, the number of actual plates = 10/0.6 = 16.7 17 actual plates 54 55 56 57 58 59 60 61 62 63