Unit Operations

Lecture 10

23 June 2010

1
 Overview
• Last time
time…
• Column Internals; sizing
• Batch (Rayleigh) Distillation
• Evaporation
E ti
• Crystallization

2
 Evaporation
Evaporate a solvent from a solution to concentrate the solution; recover the solvent, or as a
preparation for further downstream processing (like crystallization or distillation)
• Typical is removal of water or other solvents from:
o Aqueous sugar (or fructose) solutions
o Salt solutions
o Acid/basic solutions (i.e., sulfuric acid or NaOH)
o Glycerol (glycerine) solutions
o Glue
o Milk
o Fruit juices
o Vegetable extracts
o Pharmaceuticals
o Fine chemicals
• Things to consider:
o Solute concentration (initial and final)
o Solubility
l bili off the
h solute
l
o Temperature sensitivity (time/temperature)
o Foaming/frothing
o Required
equ ed T and
a dP
o Scale formation / Materials of Construction (MOC)

3
Equipment Types

4
5
6
7
Equipment Information

Perry’s 8th ed.

8
Equipment Information

Perry’s 8th ed.

9
Equipment Information

Perry’s 8th ed.

10
 Equipment
Information

Perry’s 8th ed.

11
Equipment Types

12
 Boiling Point Elevation
• So
Solute
u e insoluble,
so ub e, colloidal
co o da suspension:
suspe s o : No boiling
bo g point
po change
c a ge of
o thee solvent
so ve
• Solute soluble:
oSolute non volatile – boiling point
elevation
l i (colligative)
( lli i )
oSolute volatile – boiling point
elevation/or decrease

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 Boiling Point Elevation
• So
Solute
u e soluble,
so ub e, non
o volatile:
vo a e:
oColligative property, i.e. only depends on the number of dissolved
particles but not their composition; (from thermodynamics or charts)
oFor ideal dilute solution the boiling point rise is given by:

R  Ts2
T  K b  xdissolved   xdissolved
hs vap

where: K b is the so called ebullioscopic constant

R is the gas constant
Ts is the boiling point of the solvent
hsvap is the enthalpy of (heat of) vaporization of the solvent
xdissolved is the mole fraction of dissolve particles (moles of dissolved
particles per mole of solution, i.e. solvent for dilute solutions)
[i NaCl
[i.e. N Cl would
ld have
h 2 moles
l off dissolved
di l d particles
i l per mole
l off salt,
l since
i it
i fully
f ll dissociates]
di i ]

14
 Boiling Point Elevation
• Solute
So u e soluble,
so ub e, non
o
volatile:
• Solute soluble, and
slightly volatile:
oDetermine boiling
point elevation from
Txy diagram or

p H 2O  xH 2O H 2O PHsat2O

15
 Evaporator Model
Assumptions:
• Feed (thin-liquor) only has one
volatile solvent
• Only vaporization energy comes
f
from latent
l heat
h off vaporization
i i
of the steam
• Contents are well mixed
• Heat transfer driving force is
difference between the steam
temperature and the boiling
solution temperature T  Ts  T p 
• The P is found by knowing the
boiling point elevation of the
solution and that Tv  T p  Te
• Evaporator is well insulated

Seader & Henley, 2006 16

 Evaporator Model
Mass balance (mass units used)
m f  mv  m p
Mass balance on solute
w f m f  wv mv  w p m p

Energy balance on liquid solution

m f H f  Q  mv H v  m p H p

Energy from steam heat

Q  ms H vap
Heat transfer across the heat exchanger
Q  U A T s  T p   Q  k A Ts  T p  
Typical HT Coefficients
U (overall)
Exchanger W/m2K btu/hft2oF
Short tube vertical 1100‐2800 200‐500
Horizontal 1100 2800
1100‐2800 200 500
200‐500
Long tube vertical 1100‐4000 200‐700
Forced circulation 2300‐11000 400‐2000
Agitated film 680‐2300 120‐400
Geankoplis, 2003 Seader & Henley, 2006 17
Multiple-Effect Evaporator Systems

Seader & Henley, 2006 18

Mechanical Recompression

McCabe, Smith, Harriott, 4th ed.

19
 Overview
• Last time
time…
• Column Internals; sizing
• Batch (Rayleigh) Distillation
• Evaporation
E ti
• Crystallization

20
 Crystallization
Cool or evaporate a solution to cause crystal formation of the product in the desired (and
uniform): size, shape, and purity.

Seader & Henley, 2006

21
Thermodynamics (review)
Solid – Liquid Equilibrium

Seader & Henley, 2006

22
Thermodynamics

Seader & Henley, 2006

23
 MgSO47 H2O
Production

Seader & Henley, 2006 24

MgSO47 H2O
Production

Seader & Henley, 2006 25

 Crystals
• Crystal
y habits
• Growth
• Crystal Size Distribution (CSD)

26
Crystals (Bravais, 1848)

Seader & Henley, 2006 27

28
Crystal Systems

Seader & Henley, 2006

29
NaCl sucrose

MgS04-7H2O
30
 Crystals Habits
Includes (for example):
• Plates
• Needles
• Prisms
C depend
Can d d on things
thi like
lik growth
th
rates, nucleation, and impurities
Batch of crystals described by:
• Average
A particle
ti l size
i
Characteristic dimension
Sphericity
• Crystal Size Distribution (CSD)
Sphericity ()
surface area sphere ( with same volume ) 6  VP 
     
surface area particle ( same volume ) Dsph  SAP 

 sphere
h 1  non  spherical ti l  1
h i l particle
Seader & Henley, 2006

31
 Sphericity (exercise)
6  VP 
Fi d th
Find the sphericity
h i it off a cubic
bi particle
ti l with
ith a side
id off 5 mm.    
Dsph  SAP 

Vcube  L3  Dsph
3

Vcube  Vsphere  L  3

SAcube  6 L 2
6
Dsph  1.2407 L

6  L3 
   2    0.806
1.2407 L  6 L 

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Particle Size Measurement

Seader & Henley, 2006

33
 Particle Size
Measurement
Screens (US/British Standard Screens)
Pictures
Pi

34
 Particle Size Measurement
C lt Counter
Coulter C t L
Laser light
li ht scattering
tt i
Malvern

35
 Aperature
Crystal Size Distribution (CSD) opening  Cum. 
[mm] wt. %
Screen analysis (for example)
1 400
1.400 100
1.180 98.14
1.000 91.60
0.850 83.49
0 600
0.600 35 54
35.54
0.425 17.39
0.300 6.31
0.212 1.83
0 150
0.150 0 36
0.36
0.106 0.11
100
90
80
70

Cumulaative wt. %
60
Differential screen analysis 50
S d & Henley,
Seader H l 2006
40
30
20
10
Cumulative 0
screen 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4

analysis Screen opening [mm]

36
Questions?

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