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You are on page 1of 149

Chemical

E i

i Operations

O

i

Distillation

Dr. A

D

Anand

dV

V. P

Patwardhan

t

dh

Professor of Chemical Engineering

Institute of Chemical Technology

Nathalal M

M. Parikh Road

Matunga (East), Mumbai-400019

av patwardhan@ictmumbai edu in; avpuict@gmail

av.patwardhan@ictmumbai.edu.in;

avpuict@gmail.com;

com; avpiitkgp@gmail.com

avpiitkgp@gmail com

1

distillation:

1 Vapour liquid equilibrium

1.

2 Relative volatility

2.

3. Enthalpy

Enthalpy-Concentration

Concentration Diagram

4. Application of enthalpy

enthalpy-concentration

concentration diagram to

FLASH distillation of a BINARY mixture

5. Steam distillation

6. Differential distillation / Rayleigh distillation

(McCabe Thiele method)

(McCabe-Thiele

a) Material and energy balances

b) Determination of number of stages

c) Total reflux Fenske

Fenskess equation Minimum

number of stages

d) Minimum reflux ratio

(Ponchon Savarit Method)

(Ponchon-Savarit

a) Determination of number of stages

b) Minimum reflux ratio

c) Total reflux

MORE VOLATILE COMPONENT(s) from LESS

VOLATILE COMPONENT(s) by PARTIAL

VAPORISATION followed by condensation.

VAPORISATION,

condensation

Distribution of components in two phases = function of

(vapour-liquid equilibrium).

Distillation column consists of:

Column

C

having

i trays or packing

i and suitable

i

internals

i

Reboiler

Condenser

5

Feed enters at a suitable point.

Reboiler partially vaporises the liquid received from

the column bottom.

bottom

Vapour flows UP through the trays (or packing),

packing) leaves

at the column top and enters into overhead condenser.

A part of the condensate is withdrawn as TOP

PRODUCT,, and the rest is fed back to the column as

REFLUX that flows down the trays (or packings).

6

DOWNFLOWING liquid

liq id occ

occurs

rs on the trays

tra s (or

packing).

EXCHANGE of mass takes place between the liquid

and vapour phases: M

M.V.C.

V C from liquid vapour;

L.V.C. from vapour liquid.

Typical

di till ti

distillation

column

Vapour

3

4

F

Feed

Steam

Condensate

Reflux

1

L and V)

D: Distillate or top product

W: Bottom product

1: Distillation column

2: Feed preheater

3: Condenser

4: Reflux drum

5: Reboiler

5

W

Vapour-Liquid Equilibrium

Under a given set of conditions, the equilibrium vapour

composition is related to the liquid composition.

Gibb's Phase Rule

F

where C

number of components

number of phases

degrees of freedom

Example

Aqueous solution of C2H5OH in a closed vessel fitted

with a valve

Boiled for some time to expel the air contains only

H2O + C2H5OH

Vessel put in a constant temperature bath for sufficient

time

System

y

reaches equilibrium

q

L and V compositions,

p

,

and PT in the vapour space attain unique constant

values

10

Number of Phases = 2 (L and V)

Degrees of Freedom = 2

Total number of parameters = 4 (T, PT, L

composition V composition)

composition,

2 of these 4 parameters can be fixed to define

system COMPLETELY

11

essential for reliable design of a distillation column.

col mn

If the experimental data are not available

(multicomponent systems), a suitable predictive method

can be adopted

adopted, for example

example, UNIFAC method.

method

If data for prediction is also not available

available, conduct

experiments to determine the VLE.

12

TB

M1

H

VAPOUR

N1

T-y

(dew point)

H1

M

G

Tx

T-x

(bubble point)

LIQUID

V

L1

zF

a

V1

TA

G1

Diagonal

y=x

Equilibrium (xy) diagram

(0, 0)

13

composition

iti T-x

T (bubble

(b bbl point)

i t) curve

At constant P: Boiling Temperature versus vapour

composition T-y (dew point) curve

Liquid at Point G heated gradually Point M

heating continued Liquid becomes progressively

POORER in A

Liquid

q

Boiling

g Point ((bubble p

point)) increases

Last liquid

q

droplet

p at M1

14

Final VAPOUR at N1

further heating gives SUPERHEATED vapour

Same description can be given for LV, L1V1, G1H1

15

fraction)

L = amount of liquid,

liquid kmol (x = mole fraction)

V = amount of vapour,

vapour kmol (y = mole fraction)

Overall mole balance: F = L + V

Component A balance: F zF = L x + V y

y * z

L

length

g of section VF

F

Eli ti F :

Elimating

V

z x length of section FL

F

Lever Arm Rule

16

Sol tions:

Solutions:

p

P v and p

A A

B

Total p

pressure

x Pv 1 - x Pv

A A

A B

Pv

B B

P

A T

Pv

A A

1 - x

Pv

A B

PT

equilibrium data for IDEAL BINARY mixtures.

17

POSITIVE deviation: a liquid mixture exerting an

equilibrium total vapour pressure more than that

computed by ideal equation.

NEGATIVE deviation: a liquid mixture exerting an

equilibrium total vapour pressure less than that

computed by ideal equation.

18

AZEOTROPES

LARGE POSITIVE deviation from ideality: vapour

pressures of A and B are not much different

different, the

TOTAL PRESSURE CURVE may have a MAXIMUM

at a certain liquid composition constant boiling

mixture minimum boiling AZEOTROPE.

x-PT and y-PT curves touch at Azeotropic Composition.

x-T and y-T curves pass through a common minimum.

The equilibrium curve crosses the diagonal line at the

azeotropic

p composition.

p

19

Equiliibrium prressure

x-PT curve

x-PB curve

x-PA curve

Ideal

behaviour

y

Azeotropic

point, x = y

(0, 0)

20

press res of indi

pressures

individual

id al components are < ideal values,

al es

the TOTAL PRESSURE CURVE may have a

MINIMUM at a certain liquid composition constant

boiling mixture MAXIMUM boiling AZEOTROPE.

x-PT and y-PT curves touch at Azeotropic Composition.

x-T and y-T curves pass through a common minimum.

The equilibrium curve crosses the diagonal line at the

azeotropic

p composition.

p

21

RELATIVE VOLATILITY

Relative volatility of a component A in a mixture

indicates the EASE of its SEPARATION from another

component B.

y of A

Relative volatility

y 1 y y 1 x

AB x 1 x x 1 y

x

y

1 1 x

22

terms of vapour

apo r pressures

press res of the components:

p P

p P

y 1 y

A

T

B

T

x 1 x

p

Pv

p

Pv

A A

B B

P v vapour

p

p

pressure of A

A

v

vapour pressure of B

P

B

23

Hydrocarbons of a homologous series are nearly ideal

solutions.

For an IDEAL solution, we can write:

i

n

y P p x P v and P p

j T

j

j j

T

i

i 1

v

x P

p

j j

i

y

j P

i n

v

T

x

P

i i

i 1

where

h

P v = vapour pressure off pure componentt j

j

24

ij

i

j

x

x

j

j

y

j

in

x

1 in

v

i ij

x

P

v

i1

i

i

Pj i 1

F hydrocarbon

For

h d

b mixtures,

i

a quantity

i called

ll d equilibrium

ilib i

vaporisation ratio is extensively used:

Pv

K i i

i x

P

i

T

y

25

At equilibrium, the FUGACILITIES of component i in

the vapour phase and in the liquid phase are EQUAL.

fV fL

i

i

V

V

L

L

0

f F y P and f F x P x g f

i

i i T

i

i i T

i i i

where,

F V fugacity coefficient of component i in vapour

i

g activity coefficient of component i in liquid

i

f 0 fugacity

g

y of component

p

i at standard state

i

26

standard state can be appro

approximated

imated to the vapour

apo r

pressure at the given temperature, that is:

L

v

f x P

i

i i i

Thus, at equilibrium : V y P x P v

i i T

i i i

27

ENTHALPY-CONCENTRATION DIAGRAM

Change in composition is accompanied by a change

in enthalpy. For a given T and concentration x of a

liquid, the molar enthalpy HL can be calculated using

the equation:

HL = molar enthalpy of solution at T, kJ/kmol

CPS = specific heat of solution, kJ/(kg K)

Mav = average molecular weight of solution

T0 = reference temperature, K

HS = heat

h t off solution

l ti att T0, kJ/kmol

kJ/k l

28

ENTHALPY-CONCENTRATION DIAGRAM

Since the heat of mixing of the vapour is negligible,

we can use the following equation to compute the

molar enthalpy of the saturated vapour HV at a

given T and y:

HV = y MA {cPA (T T0) + A}

+ (1 y) MB {cPB (T T0) + B}

cPA, cPB = specific heats of pure LIQUIDS A and B,

kJ/(kg K)

A, B = heats

h t off vaporisation

i ti off A and

d B att

temperature T, kJ/kg

29

Aceone (A)-Water (B) system at 1 atm total P. Integral heat of solution (15 0C) at

different concentrations

concentrations, specific heat of solutions and xx-yy data are given:

T, 0C

HS

cPS

56.5

0.54

57

0.95

0.963

0.56

57 5

57.5

09

0.9

0 935

0.935

10

10.55

55

0 56

0.56

58.2

0.8

0.898

23.88

0.61

58.9

0.7

0.874

41.11

0.66

59.5

0.6

0.859

60.3

0.7

60

0.5

0.849

83.56

0.75

60 4

60.4

04

0.4

0 839

0.839

121.5

121 5

08

0.8

61

0.3

0.83

171.7

0.85

62.2

0.2

0.815

187.7

0.9

66.6

0.1

0.755

159.7

0.96

75.7

0.05

0.624

106.8

0.98

91 7

91.7

0 01

0.01

0 253

0.253

22.2

22 2

100

acetone = 0.57

0 57 kcal/(kg K)

Specific heat of water = 1

kcal/(kg K)

Heat of vaporisation of acetone =

A = 128.8 (T 0C 50), kcal/kg

Average heat of vaporisation of

water = B = 550 kcal/kg

30

15000 kcal/mol

(HV)2

F

W

y HV curve

y-H

N

J

Tie Lines

(HV)1

x-HL curve

(a)

x y

x,

(b)

y

R

(0, 0)

31

ENTHALPY-CONCENTRATION DIAGRAM

The amount of vapour and liquid phases SEPARATED

can be determined by Lever Arm Rule

Rule.

Point R on x-y diagram corresponds to Tie Line WD.

WD

Point Q on x

x-y

y diagram corresponds to Tie Line IJ.

IJ

Consider 2 solutions whose states (H and x or y) and

amounts are given by M and N. After MIXING, the

resultant solution is P. Hence,,

32

Component A balance: M zM + N zN = P zP

Enthalpy balance: M HM + N HN = PHP

Eliminating P: M/N = (zN zP)/(zP zM)

Eliminating P: M/N = (HN HP)/(HP HM)

(HN HP)/(zN zP) = (HP HM)/(zP zM)

Slope of section NP = Slope of section MP

Points M, N, and P are collinear.

33

FLASH

di ill i

distillation

unit

Feed

F zF , HF

F,

Vapour

Baffles

Top product

D, xD = yD , HD

Flash drum

+Q

Bottom product

W, xW , HW

34

If a sufficiently hot liquid is THROTTLED into a

vessel a part of it vaporises vapour will be richer in

vessel,

MVC partial separation.

The liquid is heated under Pressure, and throttled into

a vessel under Reduced pressure

pressure.

Let the Flow Rate, Composition, Enthalpy of FEED,

DISTILLALATE (TOP), and BOTTOM products be

((F,, zF, HF), (D,

( , xD, HD), (W,

( , xW, HW), and Q be the rate

of supply of heat exchanger:

35

Component A balance: F zF = D xD + W xW

(D + W) zF = D xD + W xW

Enthalpy balance : F HF + Q = D HD + W HW

Q

H H

x

z

D F F

W

D

F

Eliminating F :

Q

D x z

W

F H H

W F F

36

En

nthalpy (H

HL, HV),

kcal/km

mol

15000 kcal/mol

y-HV

F (z

( F, HF + Q/F)

(a)

x-HL

W

F1

x y

x,

1

P

(b)

F (zF, zF)

x z

W

F

Slope =

D

x

z

D

W

F

(0, 0)

37

Cold feed at F1 passes through preheater receives

Q heat energy hot feed F FLASHES into vapour

(D) and liquid (W) upon throttling into the flash drum.

The enthalpy and composition of vapour (D) and liquid

(W) streams are obtained by drawing TIE LINE

through F.

The point F(zF, zF) is located on the diagonal of x-y

p

plot.

38

the slope of the line FP = W/D.

W/D The line FP is the

operating line for flash vaporisation process.

By using the H-x-y and x-y curves, the amounts and

compositions of D and W can be calculated for a given

feed for given Q.

Alternatively, if the fraction of feed to be vaporised is

specified, the required Q can be computed.

The analysis

y can be extended to the case of a real stage

g

with a given value of stage efficiency (How ?).

39

STEAM

DISTILLATION

unit

it

Vapour

Receiver

Feed

B

(water)

Steam

coil

Open

steam

Steam

St

sparger

Residue

40

Steam Distillation

For an ideal binary solution, yA = pA/PT = (xA PAV)/PT

However, if A and B are IMMISCIBLE, their mixture

exerts a vapour pressure = (vapour pressures of

individual components).

Hence the BUBBLE POINT of such a mixture < boiling

point of either A and B.

Process: Live steam is p

passed through

g a liquid

q

A

vaporises leaves WITH steam condenser 2

y

((A and B)) separated

p

by

y decantation.

layers

41

Separation of high boiling materials (decolourisation,

deodourisaion of vegetable oils,

oils purification of essential

oils).

Separation and purification of hazardous materials like

turpentine

Separation of thermally unstable materials

Separation

p

of volatile impurities

p

from waste water

(removal of ammonia, VOCs)

42

PT = PAV + PBV PBV = PT PAV

If mA moles of A are volatilised by putting in mB moles

of steam

steam, and if the system operates at equilibrium

equilibrium,

mA = mB PAV/(PT PAV)

However,, if the system

y

does not operate

p

at equilibrium,

q

,

pA < PAV

43

pA/PAV

mA = mB E PAV/(PT PAV)

The above equation can be used to compute the steam

requirement.

The vaporisation efficiency usually ranges from 60% to

90%.

44

(Differential Distillation / Rayleigh

Ra leigh Distillation)

Cooling

water

L, LA, x

Kettle

(still)

yD,ave

Steam

45

Feed is charged to a still pot.

Heat is continuously supplied.

As boiling continues, MVC in liquid decreases with

time

Vapour is led to condenser

The condensate ((top

pp

product)) is collected in a receiver.

At the beginning,

g

g, the condensate is veryy rich in MVC.

46

Applicable when the components greatly differ in

volatility and when ultra

ultra-pure

pure products are NOT

required.

47

Analysis is based on differential mass balance.

Let, at instance of time,

LB(t) = moles of B at any time t left in kettle liquid

L = total moles of liquid left in kettle at time t, LA(t) +

), having

g mole fraction x

LB((t),

dL = moles of liquid

q

vapourised

p

between time t and t+dt

48

dD = moles of condensate accumulated between time t

and t+dt

x(t) = mole fraction of A remaining in kettle at time t

y(t) = instantaneous mole fraction of vapour produced

49

bet een time t and t + dt,

between

dt

dD = dL

dL (total balance)

Moles of A evaporated can be given by

by,

dLA = d(x L) = x dL + L dx

The mole fraction of vapour

p

p

phase will be computed

p

as

follows, only on the basis of dLA, because y(t) =

p

p

produced,,

instantaneous mole fraction of vapour

50

y

t t l moles

total

l vapourised

i d between

b t

ti

time t and t+dt

d Lx

xdL Ldx

y

y

ydL xdL Ldx

dL

dL

dL

dx

Ldx ydL xdL Ldx dL y x

dx

L

y x

If distillation starts with F moles of feed (xF), and

continues till the liquid reduces to W moles (xW),

) above

equation is integrated as:

x

W dL

W dx

dx

L

y

F

x

F

51

F dx

F

ln

... Rayleigh

a leigh eeq

quation

W x yx

W

If x-y data is available, the RHS can be solved

g p

graphically.

y

If y = f(x)

( ) is available, RHS can be solved analytically

y

y/

numerically.

If = Ave, then RHS can be solved analytically, as

follows:

52

W

F

dx

ln

x

W x

x

F 1 1 x

x 1 x

1 x

1

F

W

W

ln

ln

1 x

1 x

1 x

W

F

F

Fx

F 1 x

F

F

ln

ln

Wx

W 1 x

W

W

53

The AVERAGE composition of the ACCUMULATED

distillate is given be TOTAL and COMPONENT

material balances:

Total material balance: F = Dfinal + W

Component material balance:

54

Continuous Multistage

Fractional Distillation of

Binary Mixtures

55

Rec

ctifying

g

se

ection

Feed

F, zF , HF

Vapour

QC

1

n

Striipping

sec

ction

m

N

Ln

xn

HL,n

Vn+1

yn+1

HV,n+1

Envelope 1

Envelope 2

Top

pp

product

D, xD, HD

Lm Vm+1

xm

ym

m+11

HL,m HV,m+1

Envelope 3

Envelope 4

Vapour

+QB

Bottom product

W, xW , HW

56

The determination of number of stages is based on

steady state M & E B equations over the ENVELOPES

as shown in the Figure.

L & V: liquid and vapour flows ABOVE the feed

location.

location

L

L &V

V:: liquid and vapour flows BELOW the feed

location.

Ln & Vn = molar liquid and vapour flow rate LEAVING

nth stage.

g

57

LEAVING nth stage.

stage

L0 = flow rate of reflux to the top stage (suffix 0

signifies that the stream is as if coming from a

hypothetical 0th stage above top stage.

stage

QC = heat removal rate from overhead condenser.

condenser

QB = heat supply rate to reboiler (to vaporise a part of

the liquid leaving the bottom stage).

F = feed rate to the column.

58

D = rate of distillate removal from reflux drum.

xD = mole fraction of MVC in distillate.

W = rate of bottom product removal from reboiler.

xW = mole fraction of MVC in bottom product.

L0/D = R = reflux ratio.

59

Stage 1

QC

Envelope 1

Top product:

D, xD, HD

60

ENVELOPE 1

( d

(condenser

+ reflux

fl drum)

d

)

Overall

O

ll balance:

b l

V1 = L0 + D = R D + D = D (R + 1)

Component A balance:

V1 y1 = L0 x0 + D xD

Enthalpy balance:

V1 HV1 = L0 HL0 + D HD + QC

QC = D { (R + 1) HV1 R HL0 HD }

Pl

Please

note:

t y1 = xD = x0 (for

(f ttotal

t l condenser)

d

)

61

Vapour

QC

Envelope 2

Rectifying

section

Stage n

Top product

D, xD, HD

Ln Vn+1

xn ynn+11

HL,n HV,n+1

62

ENVELOPE 2

(

(part

off rectifying

if i section

i + condenser)

d

)

Overall

O

ll balance:

b l

Vn+1 = Ln + D

Component A balance:

Vn+1 yn+1 = Ln xn + D xD

Enthalpy

E

th l b

balance:

l

Vn+1 HV,n+1 = Ln HL,n + D HD + QC

If you put n = 0, equations for Envelope 1 are obtained !

63

S

Stripp

ping

sectiion

Stage m

Lm Vm+1

xm ym+1

+1

HL,m HV,m+1

Envelope 3

Vapour

+QB

Bottom

B

tt

product

d t

W, xW, HW

64

ENVELOPE 3

(

(part

off stripping

i i section

i + reboiler)

b il )

Overall

O

ll balance:

b l

Lm = Vm+1 + W

Component A balance:

Lm xm = Vm+1 ym+1 + W xW

Enthalpy

E

th l b

balance:

l

Lm HL,m + QB = Vm+1 HV,m+1 + W HW

65

Vapour

Q

QC

Rectifying

section

Feed:

F,, zF, HF

Top product:

D xD, HD

D,

Feed

stage

Stripping

section

Envelope 4

Vapour

+QB

Bottom product

W, xW, HW

66

ENVELOPE 4

( i column

(entire

l

+ condenser

d

+ reboiler)

b il )

Overall

O

ll balance:

b l

F=D+W

Component A balance:

F zF = D xD + W xW

Enthalpy

E

th l b

balance:

l

F HF + QB = D HD + W HW + QC

67

p rified b

purified

by discarding the LVC into the

downflowing liquid MVC concentration in

vapour is more than that in the feed Rectifying

OR enriching section.

Below the FEED POINT: MVC is removed or

stripped out of the downflowing liquid MVC

concentration in vapour is less than that in the feed

stripping section.

68

Feed ma

may be L,

L V,

V or V+L (two-phase).

(t o phase)

Required degree of separation: requirement of

QUALITY or PURITY.

Reflux ratio and the condition of the reflux: The ratio of

reflux FED BACK to the top and the top product

WITHDRAWN. Reflux may be SATURATED liquid or

SUB-COOLED

SUB

COOLED liquid.

69

the column:

col mn: operating press

pressure

re also determines the

TEMPERATURE of column.

P = f(type, number of hydraulic design of trays OR

type and size of packings)

packings).

P is very important if the column is run at

LOWER PRESSURES.

Tray / packings type: determine the efficiency of

separation.

p

70

Developed in 1925: graphical solution of material

balance equations together with the equilibrium

relation x-y (or equilibrium data).

ASSUMPTIONS:

vapour) from one tray to another over any section of

the distillation column, that is:

L0 = L1 = L2 = ... = Ln = L (RECTIFYING section);

Lm = Lm+1 = ... = LN = L (STRIPPING section) 71

AND

V1 = V2 = V3 = ... = Vn+1 = V (RECTIFYING section);

Vm+1 = Vm+2 = ... = VN+1 = V (STRIPPING section)

2. Heat loss from distillation column is negligible. (If

there are heat losses,

losses there will be NET condensation

within the column, leading to a corresponding variation

in the flow rates along the column.

72

Steps:

(1) Draw equilibrium curve using available x-y data

(2) Draw operating lines for the rectifying and the

stripping sections

(3) Draw the STEPS between the equilibrium curve

and the operating lines to find out the number of

IDEAL stages.

73

ENVELOPE 2 (part of rectifying section + condenser)

Component A balance: Vn+1 yn+1 = Ln xn + D xD

L

L

0

Since R

D D

x

L

D

LD

x D

y

x x

n1 V n V D V D n V D

y n 1

xD

R

xn

R1

R1

74

Slope = R/(R+1)

Y-intercept = xD/(R+1)

The line satisfied by xn = xD; yn+1 = xD

This equation is called the operating line for

RECTIFYING section

section..

75

ENVELOPE 3 (part of stripping section + reboiler)

Component A balance: L xm = V ym+1 + W xW

Since V L W

L

W

y

x

x

m 1 V m V W

L

W

y

x

x

m 1 L W m L W W

76

Slope = L/(LW)

The line satisfied by xm = xW; ym+1 = xW

This equation is called the operating line for

STRIPPING section

section.

77

Consider the plate ON WHICH the feed is introduced

(feed plate).

plate)

L,, HL,f1

L f1 V, HV,f

Vf

F, zF,

HF

L, HL,f V, HV,f+1

78

Enthalpy balance:

F HF + L HL,f1 + V HV, f+1 = L HL,f + V HV,f

Assuming Uniform Enthalpy:

and HV,f+1

V f+1 HV,f

V f HV

HL,f1 HL,f HL

F HF + L HL + V HV = L HL + V HV

((L L)) HL = ((V V)) HV + F HF

79

Eliminating V and V,

L L H V H F

q say

F

H H

V

L

heat required to convert 1 mole of

FEED to saturated vapour

q

heat required to convert 1 mole of

SATURATED FEED to saturated vapour

FEED to saturated vapour

of the saturated liquid

80

stage as a res

result

lt of introd

introduction

ction of the feed

LIQUID FRACTION in the feed

FEED to

t saturated

t t d vapour

Also, q

molar heat of vaporisation

of the saturated liquid

Feed at its dew point (saturated vapour): q = 0

If feed is a two-phase mixture, q = fraction of liquid in

the feed (1 q) = quality of the feed

81

operating line and STRIPPING operating line is (x,

( y),

)

then:

V y = L x + D xD and V y = L x W xW

Subtracting the above equations, and using the equation

for component balance for the complete column (F zF =

D xD + W xW), we get:

(V V

V)) y = (L L

L)) x + (D xD + W xW) = (L L

L)) x + F zF

Total material balance on feed plate:

p

F + L + V = L + V

82

wee get the equation

eq ation of FEED LINE:

z

q

y

x F , passing

i through

h

h z ,z

F F

q 1

q1

and the intersection of two

two ope

operating

rating lines

83

(staircase) constr

construction

ction bet

between

een the equilibrium

eq ilibri m curve

c r e

and operating lines.

(xn, yn): on equilibrium curve.

(xn, yn+1): on operating line.

Construction may start from either D (xD) or W (xW).

When the FEED LINE is crossed, a CHANGEOVER

from one operating

p

g line to the other is done (that is, a

transition from RECTIFICATION to STRIPPING

section,, or vice versa).

)

84

(q < 0): Explain.

2 If feed

2.

f d is

i Saturated

S t

t d Vapour:

V

f d line

feed

li is

i horizontal

h i

t l

(q = 0): Explain.

3. If feed is Liquid + Vapour: feed line has VE slope

(0 < q < 1): Explain.

Explain

4 If feed is Saturated Liquid: feed line is vertical

4.

(q = 1): Explain.

5. If feed is Subcooled Liquid: feed line has +VE slope

(q > 1): Explain.

85

4

3

Subcooled L

( ))

(+,

V+L

(, +)

2

Saturated L (, )

F

Saturated V ((0, +))

1

Superheated

S

h t dV

(+, +)

L L H V H F

q

F

H H

V

L

z

q

x F

Feed line: y

q1

q1

86

D

N

M

S

E

Feed =

S

Saturated

Liquid

i i

W

87

TOTAL REFLUX

If the liquid from overhead condenser is TOTALLY

recycled to the column (D = 0),

0) the column is said to

run at total reflux. Also no product is drawn from

the reboiler either there should not be any Feed.

Feed

R = L0/D = L0/0 =

Operating line for Rectifying section

x

R

D

y

x

n1 R 1 n R 1

When R , Slope 1, Y-intercept 0

Operating line coincides with DIAGONAL

88

infinite R are minimum.

minim m

Total reflux is very often used during the startup of a

distillation column till the steady state is attained.

After this, continuous flow of feed, top product, and

bottom product withdrawal are

SIMULTANEOUSLY started.

89

Fenskes equation

Used to compute theoretically the minimum number of

trays if the relative volatility remains reasonably (more

or less) constant. It also assumes a total reboiler

(analogous to total condenser)

condenser).

If w is relative volatility of A at the reboiler

temperature, and xW, yW are Liquid and Vapour mole

fractions in the reboiler, then:

y

x

W

W

W 1 x

1 y

W

W

90

tra (Nm) has a mole fraction yW of component A

tray

A. The

Liquid leaving this tray has a composition xNm (xNm,

yW) lies on the Operating Line xNm = yW. Therefore,

Therefore

the above equation can be rewritten as:

x

x

Nm

W

W 1 x

1 x

Nm

W

Applying the same procedure to the case of tray number

Nm, we get:

y

x

x

Nm

Nm

W

Nm 1 x

Nm W 1 x

1 y

Nm

Nm

W

91

xD),

) wee get:

x

x

y

W

D

1 ...

1 2

Nm 1 Nm W 1 x

1 x

1 y

D

1

W

N 1 x

x

m

W

D

average

1 x

1 x

D

W

1

x

D

W

log

1 x

x

W

D

N 1

m

log

average

g

92

which

hich is useful

sef l for the calculation

calc lation of MINIMUM

number of trays.

93

This is exactly analogous to the (L/G)min for gas

absorption. This is based on the identification of

pinch point.

Locate the points D (xD, xD) and W (xW, xW) on the

DIAGONAL of the x-y diagram. These are the

terminal points of operating lines.

Draw the feed line through

g F from the known feed

composition zF, and feed quality (given by q); locate the

point of intersection of the feed line and the

p

equilibrium curve (x-y diagram). Call this point M. 94

e tend this line till the Y-axis.

extend

Y a is

Y

Y-intercept

intercept = E = xD/(Rm + 1).

1) Get Rm from the

intercept.

At Reflux Ratio = Rm, the number of stages for the

given separation are infinity (driving force becomes

ZERO at the PINCH POINT).

95

D

M

F

Slope = Rm/(Rm + 1)

Yi t

Y-intercept

t = xD/(Rm + 1)

W

96

Sieve Tray

97

Tray Columns

98

Tray Deck

99

Reboilers

100

Reboilers

Bottom

Tray

Bottom

Tray

Heating

Medium

Heating

Medium

Bottoms

Product

Bottoms

P d t

Product

Circulating Pump

Forced Circulation

Vertical Thermosiphon

101

Reboilers

Bottom

Tray

Bottom

Tray

Heating

Medium

Bottoms

Product

Kettle

Heating

Medium

ed u

Bottoms

Product

Horizontal Thermosiphon

102

Feed Distributors

103

The Real

Real World

104

The Real

Real World

Plugged Distributor

Tray Blanking Strips

105

106

107

108

Structured Packings

Fair, J.R., Seibert, A.F., Behrens, M., Saraber, P.P., and Olujic, Z. Structured Packing

Performance Experimental Evaluation of Two Predictive Models, Industrial and

Engineering Chemistry Research 2000,

2000 39,

39 1788-1796.

1788-1796

109

110

Calculations on an Enthalpy-Concentration (H-x-y)

diagram.

diagram

If the dew point and bubble point lines are more or less

straight and roughly parallel Latent heat of

vaporisation is basically constant with respect to

composition Prerequisite for constant molar

overflow, energy balances may be neglected.

If the saturation curves show significant

g

changes

g in

curvature constant molar overflow cannot be

assumed.

111

constr ction beca

construction,

because

se it takes direct account

acco nt of the

thermal effects and does not require an assumption of

constant equimolar overflow.

overflow

Feed and product points (F,

(F D,

D W) can be located on Hx-y diagram. The coordinates are their composition

and enthalpy

enthalpy.

112

Rec

ctifying

g

se

ection

Feed

F, zF , HF

Vapour

QC

1

n

Striipping

sec

ction

m

N

Ln

xn

HL,n

Vn+1

yn+1

HV,n+1

Envelope 1

Envelope 2

Top

pp

product

D, xD, HD

Lm Vm+1

xm

ym

m+11

HL,m HV,m+1

Envelope 3

Envelope 4

Vapour

+QB

Bottom product

W, xW , HW

113

The determination of number of stages is based on

steady state M & E B equations over the ENVELOPES

as shown in the Figure.

L & V: liquid and vapour flows ABOVE the feed

location.

location

L

L &V

V:: liquid and vapour flows BELOW the feed

location.

Ln & Vn = molar liquid and vapour flow rate LEAVING

nth stage.

g

114

LEAVING nth stage.

stage

L0 = flow rate of reflux to the top stage (suffix 0

signifies that the stream is as if coming from a

hypothetical 0th stage above top stage.

stage

QC = heat removal rate from overhead condenser.

condenser

QB = heat supply rate to reboiler (to vaporise a part of

the liquid leaving the bottom stage).

F = feed rate to the column.

115

D = rate of distillate removal from reflux drum.

xD = mole fraction of MVC in distillate.

W = rate of bottom product removal from reboiler.

xW = mole fraction of MVC in bottom product.

L0/D = R = reflux ratio.

116

Stage 1

QC

Envelope 1

Top product:

D, xD, HD

117

ENVELOPE 1

( d

(condenser

+ reflux

fl drum)

d

)

Overall

O

ll balance:

b l

V1 = L0 + D = R D + D = D (R + 1)

Component A balance:

V1 y1 = L0 x0 + D xD

Enthalpy balance:

V1 HV1 = L0 HL0 + D HD + QC

QC = D { (R + 1) HV1 R HL0 HD }

Pl

Please

note:

t y1 = xD = x0 (for

(f ttotal

t l condenser)

d

)

118

Vapour

QC

Envelope 2

Rectifying

section

Stage n

Top product

D, xD, HD

Ln Vn+1

xn ynn+11

HL,n HV,n+1

119

ENVELOPE 2

(

(part

off rectifying

if i section

i + condenser)

d

)

Overall

O

ll balance:

b l

Vn+1 = Ln + D

Component A balance:

Vn+1 yn+1 = Ln xn + D xD

Enthalpy

E

th l b

balance:

l

Vn+1 HV,n+1 = Ln HL,n + D HD + QC

If you put n = 0, equations for Envelope 1 are obtained !

120

S

Stripp

ping

sectiion

Stage m

Lm Vm+1

xm ym+1

+1

HL,m HV,m+1

Envelope 3

Vapour

+QB

Bottom

B

tt

product

d t

W, xW, HW

121

ENVELOPE 3

(

(part

off stripping

i i section

i + reboiler)

b il )

Overall

O

ll balance:

b l

Lm = Vm+1 + W

Component A balance:

Lm xm = Vm+1 ym+1 + W xW

Enthalpy

E

th l b

balance:

l

Lm HL,m + QB = Vm+1 HV,m+1 + W HW

122

Vapour

Q

QC

Rectifying

section

Feed:

F,, zF, HF

Top product:

D xD, HD

D,

Feed

stage

Stripping

section

Envelope 4

Vapour

+QB

Bottom product

W, xW, HW

123

ENVELOPE 4

( i column

(entire

l

+ condenser

d

+ reboiler)

b il )

Overall

O

ll balance:

b l

F=D+W

Component A balance:

F zF = D xD + W xW

Enthalpy

E

th l b

balance:

l

F HF + QB = D HD + W HW + QC

124

Rectifying Section

ENVELOPE 2 (part of rectifying section + condenser)

Total material balance: Vn+1 = Ln + D

Component A balance: Vn+1 yn+1 = Ln xn + (Vn+1 Ln) zD

Ln / Vn+1 = (zD yn+1) / (zD xn)

Note: Reflux may be a sub-cooled liquid and hence the

composition

p

is denoted by

y zD.

125

Energy balance:

Vn+1 HV, n+1 = Ln HL,n + D (HD + QC/D) = Ln HL, n + D QD

where QD = Enthalpy removed from the TOP section of

the column per mole of distillate.

distillate

Substituting D = Vn+11 Ln :

Vn+1

QD

+1 HV,

V n+1

+1 = Ln HL,

L n + (Vn+1

+1 Ln) Q

Ln/Vn+1 = (Q

(QD HV,

(Q D HL,

V n+1))/(Q

L n)

The q

quantity

y Ln/Vn+1 is called internal reflux ratio.

126

Q H

z y

D

V,n 1

D

n

1

z x

Q H

D n

D

L,n

Q H

Q H

D

Ln

L,n

D

V

V,n

n1

z x

z y

D n

D

n1

,

The 3 points z , Q , x , H

D

D n

L,n

and y

,H

, are COLLINEAR.

V,n 1

V,

n1

the points Ln , Vn 1 , and QD are COLLINEAR.

127

obtained by

b subtracting

s btracting Ln from Vn+1.

However

However, NONE of the phases can have the

composition zD, and enthalpy QD = HD + QC/D.

The stream D is a fictitious stream defined for the

purpose of graphical construction.

D lies vertically

y above D,, because they

y have same

abscissa = zD.

128

Put n = 0 D, D, V1 are collinear.

Point L1 (x1, HL1) is located by drawing a tie line from

V1.

L1D

D is joined to get point V2, and so on

129

Q H

Q H

V

D

V,n 1

D

L,n

n

n

1

Now:

V

Q H

L

Q H

n1

D

L,n

n

D

V,n 1

Q H

Q H

L

D

V

D

L,0

D

L,0

0

1

Put n 0

Q H

L

Q H

L

0

D

V

V,1

1

0

D

V

V,1

1

Q H

D

D

D

1

L

Q H

0

D

V,1

Q H

L

vertical distance DV

D

V,1

1

R 0

D H

H

vertical distance V D

D

V,1

1

L

130

to locate D.

D

First

First, D (zD, HD) is located from the given state of the

distillate.

A vertical line through zD intersects the y-HV curve at

V1.

Then, obtain D

D so that the above relation for R is

satisfied.

131

Rectifying Section

HL , HV

y-HV curve

Vn+1

Vn

V3

V2 V1

x-HL curve

Ln

Ln1

L2

Tie lines

L1

D

00

0.0

x y

x,

zD 1.0

10

132

Stripping Section

ENVELOPE 3 (part of stripping section + reboiler)

Total material balance: Lm = Vm+1 + W

Component A balance:

Lm xm = Vm+1 ym+1 + (Lm Vm+1) xW

Ln / Vm+1 = (ym+1 xW) / (xm xW)

133

Energy balance:

Lm HL, m Vm+1 HV, m+1 = W HW QB = W (HW QB/W)

Lm HL, m Vm+1 HV, m+1 = W QW

where QW = Enthalpy supplied to the BOTTOM section

of the column per mole of bottom product.

product

Substituting D = L

Lm V

Vm+1

+1 :

Lm HL,

QW

L m Vm+1 HV,

V m+1 = ((Lm Vm+1) Q

Lm / Vm+1 = ((HV,

QW) / ((HL,

QW)

V m+1 Q

L mQ

134

H

Q

y

x

V,m 1

W

m

1

W

x x

H

Q

m

W

L,m

W

Q

Q

H

H

V m1

V,m

W

L

L,m

m

W

y

x

x x

m1

W

m

W

,

The 3 points x , Q , x , H

W W m L,m

and y

,H

, are COLLINEAR.

,

m+1 V,m+1

, and Q are COLLINEAR.

m m+1

W

135

Vm+1.

The stream W is a fictitious stream defined for the

purpose of graphical construction.

W lies vertically below W, because they have same

abscissa = xW.

V

V N+1 (reboiler vapour) should lie on the y

y-H

HV curve on

the tie line drawn from W.

136

at LN (collinearity

(collinearit condition)

condition).

The tie line through LN intersects the y-H

y HV curve at

VN, and so on

137

Stripping Section

HL , HV

VN+1

VNV

N1

y-HV curve

V1

W L

N

x-HL curve

xW

0.0

W

x, y

D

zD 1.0

Tie lines

Operating

p

g line SEGMENTS

138

Feed Plate

A changeover from one section to the other is necessary

at the feed plate,

plate and hence feed line is required.

required

Consider the material and enthalpy balances over

envelope 4, that is, entire column + condenser +

reboiler.

reboiler

Component A balance:

( D zF )

139

Enthalpy balance:

(D + W) HF + QB = D HD + W HW + QC

Q

H H C

F

D

H Q

D

D

F

Q

W

Q H

D

F

H B H

W W

F

z x

H Q

H Q

Q H

W F

W F

W D

F

F

z z

Q H

z x

z z

D F

D

F

F

W

D F

The 3 points W(xW, QW), F(zF, HF), and D(zD, QD)

are collinear.

140

feed in terms of composition and enthalp

enthalpy.

F(zF, HF) lies on the line joining D and W.

W

W

W:: a fictitious stream of flow rate W

W = L

Lm V

Vm+1.

D

D:: a fictitious stream of flow rate D

D = V

Vn+11 L

Ln.

F = D + W = D + W

Therefore, F, a real stream can be viewed as a stream

y mixingg the 2 fictitious streams D and W.

obtained by

The line DW is called feed line.

141

stages on H-x-y

H

diagram:

Data supplied (directly or indirectly): Concentrations

Concentrations,

Enthalpies, Flow Rates of Distillate, Bottom Product, as

well as Reflux Ratio.

Ratio

Points D,

D D

D, and F are located.

located

DF

D F is joined, and extended to meet the vertical line

{drawn through W(xW, HW)} at point W.

Stages can be constructed either from D or from W.

142

crossed.

crossed

The stage at which the changeover is made is feed

stage.

Construction continues till the other end point is

reached.

reached

143

stages on x-y diagram:

Draw the equilibrium curve (x-y

(x y diagram) using

separate axes below the H-x-y diagram using matching

scale.

scale

Locate (zD, zD) and (xW, xW) on the diagonal line.

line

Since any line starting from D

D and W

W intersects the H

Hx and H-y curves at xn and yn+1 respectively, the point

((xn, yn+1) is p

point on the operating

p

g line in the x-y

y

diagram.

144

each of these lines,

lines the point (x

( n, yn+1) is located on the

x-y diagram.

All these points are joined, giving rise to two curves;

these are the 2 operating curves,

curves namely,

namely rectifying

section operating curve and stripping section operating

curve.

curve

Since the flow rates in both these sections are not

constant (constant molar overflow is not applicable),

p

g lines are not straight.

g

the operating

Staircase construction g

gives the number of ideal stages.

g

145

If a line through D or W coincides with tie line, the

corresponding (x,y)

(x y) values give a pinch point.

point

Reflux ratio is given by:

Q H

vertical distance DV

D

V,1

1

R 0

D H

H

vertical distance V D

V,1

D

1

L

V1 ((or the nearer the point

p

D to the H-x

distance DV

curve), the smaller is the reflux ratio.

146

tie line thro

through

gh the feed point,

point minimum

minim m reflux

refl ratio

occurs.

However, for some highly nonideal mixtures, it may

happen that a tie line through a point other than F

intersects the vertical line (drawn through zD) at the

smallest distance

distance. In that case

case, the same should be

taken as the true pinch point.

Once (D)min has been located on the H-x-y diagram,

p

using

g the

then the minimum reflux ratio is computed

above relation.

147

Total Reflux

In this case, the reflux ratio is infinite.

Naturally, the points D and W are located at infinity.

Therefore, all the lines through D and W are vertical

lines.

lines

Locate V1 vertically

y above zD, on the H-y

y curve.

148

Draw a tie line from V1, which will intersect H-x curve

at L1.

Draw a vertical line from L1, which will intersect H-y

Hy

curve at V2.

Continue the above construction till xW is reached.

This (obviously) gives the minimum number of ideal

stages.

149

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