DISTILLATION Two-component distillation

• Two-component distillation
• Multi-component distillation
• Short-cut methods
• Rigorous methods
– Efficiency
– Column design
– Batch distillation
– Packed column for distillation
KAT / Distillation 1 KAT / Distillation 2

Two-component distillation Multicomponent distillation

• Short-cut methods based on:

– Constant relative volatilities
– Equal molar heat of vaporisation
– Negligible heat of mixture
• Methods:
– Graphical (McCabe-Thiele and H-x diagram)
– Numerical (Lewis-Sorel Method)
• Key parameters:
– Number of theoretical plates at total reflux
• Minimum number of plates
– Minimum reflux ratio, Rm
KAT / Distillation 3 KAT / Distillation 4
 Multi-component distillation Specify Operation. Degree of Freedom
Degrees of freedom = number of variables - number
• Several columns or one column with side-streams of design relationships
• Complex calculations
• Operation in a column influence the operation in ⎡Degrees of ⎤ = ⎡ Number of components⎤
Column ⎢⎣freedom ⎥⎦ ⎢⎣in feed (C) + 6 ⎥⎦
other columns
• Feedback • C+2 are always specified
– Feed composition C
– Feed rate 1
– Feed enthalpy 1
– Feed Temperature 1
– Pressure 1
KAT / Distillation 5 KAT / Distillation 6

Specify Operation. Grades of Freedom Multi-component methods

Rating methods
• Specify required separation, e.g. – purity of one or
more products – recovery of one or more Existing column determine the separation
components • Input Data:
• Four variables remain to specify, e.g., – Number of plates
– Feed location
– Flow rate for Distillate / Bottom product
– Reflux ratio
– Reflux ratio – Distillate rate / feed rate
– Number of plates
– Concentrations (two) • Output Data:
– Distillate composition
• Do not over-specify – Bottom products composition
– (Concentration and temperature profiles)
KAT / Distillation 7 KAT / Distillation 8
 Multi-component methods
Design methods Short-cut methods/ Multi-component
Given separation dimensioning the column
• Empirical relationships, assumptions:
– (Saturated reflux, constant relative volatility,
• Input Data:
– Distillate composition non-azeotropic mixture). Simple calculations
– Optimum feed stage • Rating method:
– Bottom products composition
– Design: use the minimum reflux ratio (Rm) • S-B (Smith-Brinkley). Analytical solution for
• Output Data: separation (Perry)
– Number of plates • Design method:
– Feed location
– Reflux ratio, • FUEM (Fenske-Underwood-Erbar-Maddox)
– Distillate flowrate • FUG (Fenske-Underwood-Gilliland)

KAT / Distillation 9 KAT / Distillation 10

FUEM/FUG method
FUEM/FUG method
• Step 2 Specify
– Separation of the light and heavy key component
• Step 1 Define key components:
– Reflux Ratio (actual Reflux) /(minimum Reflux)
– Light key component = lightest component in the
– Feed location
bottom product
– Heavy key components = heaviest component in • Step 3 Estimate the minimum number of ideal
the distillate plates, n - Total Reflux

⎡⎛ x ⎞ ⎛ x ⎞ ⎤
log ⎢⎜ LK ⎟ ⎜ HK ⎟ ⎥
x x
Fenske’s equ. n + 1 = ⎣⎝ HK ⎠D ⎝ LK ⎠B ⎦
LK
HK
log[α LK ,HK ]Av
KAT / Distillation 11 KAT / Distillation 12
 FUEM/FUG method FUEM/FUG method
• Step 4 Estimate minimum reflux ratio, Rm
α j,HK ⋅ x dj • Step 5 Estimate number of required ideal
Underwood’s method R m + 1 = ∑ plates, n:
j α j,HK − θ

– θ are the root of equ. CR2-11.114 – Erbar-Maddox diagram

α j,HK ⋅ x fj – Gillilands diagram (CR2 Fig 11.42)

1− q = ∑
j α j,HK − θ
Relationship between number of ideal stages, N
q = Fraction of liquid at boiling point in the feed and reflux ratio, R where Nm and Rm are
αHK< θ< αLK parameters
KAT / Distillation 13 KAT / Distillation 14

Erbar-Maddox diagram Gillilands diagram

Rm = Minimum reflux ratio
Nm = Minimum number of ideal stage, (n+1)

Line-line scale Log-log scale

KAT / Distillation 15 KAT / Distillation 16
 Rigorous methods Rigorous methods
• For each plate: • Different methods solve equations system in
– Mass balance for each components different ways.
– Energy balance • High accuracy
– Vapour-Liquid Equilibrium • Other methods (Perry, 7th Ed, 13-39)
– Other (e.g., mixtures properties) – Matrix method: Naphtali and Sandholm

• Nonlinear equation system

KAT / Distillation 17 KAT / Distillation 18

Efficiency
• Usually less than 1.0
• Vapour-liquid equilibrium is not reach in
each plate. Poor contact between the phases:
• Too large vapor flow rate
• Big bubbles
• Low liquid depth on the plate
• Poor flow distribution on the plate. Stagnant
liquid
Efficiency
• Efficiency
– Overall column efficiency
– Murphree plate or Local efficiency
not applicable for multi-component distillation
• Overall column efficiency
⎡Overall column⎤ Number of ideal plates
⎢ ⎥=
⎣⎢ efficiency ⎦⎥ Number of actual trays

KAT / Distillation 19 KAT / Distillation 20

 Overall column efficiency Overall column efficiency
• Overall column efficiency: Make sure that the plate operate properly
– Decreases with viscosity and relative volatility
(surface tension) without weeping or flooding
– May decrease slightly with vapor flow and
increases with liquid flow Misoperation such as excessive foaming,
– Dependent on geometry of the tray entrainment, weeping etc. lowers the plate
– Increases with pressure
efficiency
• Empirical relationships.
– Efficiency vs. (viscosity) • (relative volatility)
(O´Connell based on hydrocarbon – systems)
– Efficiency vs. vapour flow rate (F-factor)

KAT / Distillation 21 KAT / Distillation 22

Quick estimation of overall effciency Typical data for efficiency

KAT / Distillation 23 KAT / Distillation 24

 Azeotropic / extractive distillation Azeotropic Distillation

• Cases
– Separation of components is difficult
– Azeotropic mixture
• Azeotropic distillation
– Add en new component (entrainer) to form an
azeotrop
• Extractive distillation
– Add en new component (extractive agent) that
modify the relative volatility
KAT / Distillation 25 KAT / Distillation 26

Extractive Distillation Batch distillation

– Unequal feed
– Small amount
– Several fractions,
high purity
– The process can
be tracked

KAT / Distillation 27 KAT / Distillation 28

 Batch distillation Constant Reflux Ratio
• Methods of operation
– Constant reflux ratio
• Distillate purity decreases with time
– Constant distillate composition
• Reflux ratio must increase continuously
• Calculations (Operation varies with time)
– Short-cut methods:
• Based i Fenske-Underwood-Gilliland (FUG)
– Rigorous methods:
• Transient differential equation for each plate

KAT / Distillation 29 KAT / Distillation 30

Constant distillate composition Criteria to choose types of trays

• General aspects
– Vapor flow capacity
– Liquid flow capacity
– Flexibility
– Pressure drop
– Cost
• Operating range (CR2 Fig.11.54) for stable
operation – Operating limits
KAT / Distillation 31 KAT / Distillation 32
 Operating range - Performance diagram Types of trays

Limited
range of
vapor and
liquid
flow rates

KAT / Distillation 33 KAT / Distillation 34

Bottnar Design of colomn for distillation

• Bubble Cap Trays • Diameter determined from:

– Expensive – high pressure drop – can handle – Upper limit of vapor velocity
very low liquid flow – can handle very low • Liquid entrainment
vapor flow – large operating range • Pressure drop – flooding
• Sieve trays • Number of actual plates determined by:
– Simple construction – cheap – low pressure – Separation
drop – smaller operating range – Efficiency
• Valve Trays • Plate spacing determined from criterion:
– Rather cheap – low pressure drop – large – Extent of entrainment (Medstänkning)
operating range and flexible
– Pressure drop

KAT / Distillation 35 KAT / Distillation 36

 Distillation in Packed Columns HETP
• when the separation is easy
⎡
⎢
⎢
Smaller ⎤⎥⎥ ⇒ ⎡⎢Lower⎤⎥ ⇒ ⎡⎢⎢Higher ⎤
⎥
⎥
⎢ ⎥
⎢Packning⎦⎥ ⎣HETP ⎦ ⎢⎣Pressure drop⎥⎥⎦
⎣⎢
⎥ ⎢ ⎥ ⎢

• unsuitable for low liquid reflux

C2 αμ L
HETP = C1 ⋅ G '
C
⋅ d c3 ⋅ Z1/3
Packed bed height based on ρL
• HETP (Height Equivalent of a Theoretical Plate) G ' = Mass velocity of the vapour
d C = Column diameter
Height of packing⎤⎥⎥
⎡
⎢
HETP = ⎡ ⎣⎢ ⎦
Z = Packed height
⎢ Number of ideal stages⎥
⎤
⎢ ⎣ ⎥ ⎦
C1 , C 2 and C3 = Constants for packings
KAT / Distillation 37 KAT / Distillation 38

HETP for Full-scale Plant HTU (Height transfer unit)

Type of packing, application HETP, (m) • Number of transfer units
25 mm diam. packing 0.46
yt
38 mm diam. packing 0.66 dy kG 'a 1
NG = ∫ = Z = Z
50 mm diam. packing 0.90 y yi − y
b
G' HG
Absorption duty 1.5 - 1.8
Small columns (d< 0.6 m) Column diameter xt
dx kL 'a 1
Vacuum columns Values above + 0.1m
NL = ∫x−x =
L'
Z=
HL
Z
xb i

KAT / Distillation 39 KAT / Distillation 40

 HTU (Height of a Transfer Unit)

• Height, Z Z = H G ⋅ N G Z = HL ⋅ NL

– A low value of HG or HL corresponds to an

efficient column

• Height of an overall transfer unit

G' L'
H OG = ' H OL = '
Kg ⋅ a Kl ⋅ a

KAT / Distillation 41 KAT / Distillation 42

KAT / Distillation 43 KAT / Distillation 44

KAT / Distillation 45 KAT / Distillation 46

KAT / Distillation 47 KAT / Distillation 48