CRYSTALLTZATION

1. INTRODUCTION

- Industries in Bangladesh using crystallization

- Crystallization process
- Importance of crystallization

- Nucleation of crystals
- progress of crystallization i
- Solubility relations *I

- Crystal growth rate

- Crystal Size Distribution (CSD)
- Equiiibria and yields - McCabe, Smith & Haniott

3. CRYSTALLIZATION EQUIPMENT
Classification basis - I Foust/Ghosal
a COLLING CRYSTALLIZERS
Tank crystallizer (bath process) - Badger & Banchero
Swenson - Walker Crystallizer (continuous) - !:oust

- EVAPORATOR CRYSTALLIZERS
Salting evaporators - Foust
Forced circulation (evaporative crystallizer - Perry
Draft Tube Baffle (DTB) Crystallizer - Foust
Oslo/Krystal Crystallizer - Perry
/
a VACUUM CRYSTALLIZERS

4. DESIGN OF CRYSTALLIZER
a Heat and mass balances - Badger & Banchero
a Factors to be considered in designing crystallization Trocess- Mc Ketta
a Information required to specifjr crystallizer - Perry
a Illustrative calculations
Design of a forced type crystallizer - M.cKetta
5. CASE STUDIES
Aluminum Sulfate (Alum) - 4 large r:nmber of enterprises
Ammonium Sulfate - Femhugonj Fertilizer Factory
(NGFF)
Zinc Sulfate and Magnesium Sulfate - Wata Chemicals
Ferrous Sulfate - Pilot-plant at BCSIR
 1. INTRODUCTION
inuusrries in iirr~giacirsiiusitlY ELY ~ i a ; i i ~ a i ; U ~
- Sugar industry
- Common salt (cottage) industry
- Fertilizer production: Zinc sulfate, M a g n e ~ ~sulfate
u~~
- - Alum production .
.
- Ferrous sulfate
- (from iron turniilgs
-9pilot-plant
- at BCSIR) .-

.,
' .
Crystallization
It refers to a solid liquid separation process in which solid particles I

are formed within a homogeneous phase. I

i

Importance of crystallivtion
Crystallization is an important industrial process because of the
number of materials that are and can Be marketed in the form of I
crystals.

II Advantages of crystallization compared with &her methods of

separation are that:
-It is capable of producing very high purity products from -
impure solutions with very low energy input.
2. Often these separations can be performed in ow-step,
yielding a product of not only high purity but of g ~ ~ d
appearance with high bulk density and good handling
chamteristics.
3. -- or
Crystalline product can be dewateredesily on filter
centrifuges, and the drying requirements are minimal due to
the low moisture content of the cake leaving the filter or
centrifuge.

I TERMINOLOGY: MAGMA :Mother liquid plus crystals

CSD :Crystal size distribution
'

I CHARACTERISTICS OF
CRYSTALLINE PRODUCTS: Particle size, shape, purity and
nloisture content.
t; r"
MY)
40
 Fig- 1. ~ i . f, f e, r ~ t . w & ~ S - p 6 p .CSP
, ~ f i id~agb,(same data) , t! .-,-, , 9

--- --

I +c.>,.,
r : I

&*&Fa:
c *fi"p&ti~@ -"+i%.
\ I . , * a,..
- &'L*&i 2)! .?
T5,,a,.
3-

often ark -
. represel%~@ y ,,
ciokely - ,l)y
5 E -

F.L.the :.Ros
u54#e
jn- -+
9 og
FL%

2
-%-.
+x -
I.P;,.I

RammlerSperling-
.! ,:, ;.,
b

-l',MhQt~,".>-
.-IiCxC,
;qrr-
: .73
Y

.u- -
i ~ k ?equation:.
) in4

where,,.'* i 0 - 50 98Q I50'

.@$Miiiih
4

..- ..=:diameter
*h.-,.,.,m J d c. f

d tl?!!.'~ ' Fjqpew L*

. = mean- diametei
? tk$tjl #-):-i)*_.~~

dip u , ..I L.- .+&+

f 4*3q .#.

-n = @nifo?mitY ,, factor
*..+ , t'r t I ,-,~d e

T~Fgreat@'"' . &a more

MW.~*IIC-%<
nearly
Y b t %
&2
uniform
*. ' . ,
-"-,,.
#&t~&"~i$fnnb
d m w y
t l l . C 1 * , I 1 + , I =
L

3f
;-'w*b,&

< ' 1
 - -
. n , ..r - ,

I
\
-.. . . . .

..
Mesh seporOfOr

-
-- - - - L
 .
COOLING
WATER

i Figu e 19.23. Swetison-Walksr crystallizer. (Courtesy

f Swenson Division of Whiting Corporation.;
Fa-7-
- .
Figure 19.24. "Krystal" crystallizer fw production of
ammonium~sulfate.(Courtesy Struthen-WeNr Corp.) +sun
 Propeller

\
TO barometric
condenser +if?-- drive

Elutriation
Circulation Pump

Figure 19.26. A draft-tube-baffle vacululm crystal-

lizer. Note internal fines sesaration and crvstal
 ... 1. '

Me &e- $-'LA

Burome tric condenser

 Example 11-2. r eA
z -S is to be used to produce I ton/hr of

A
cogperas . FeS04=7Hz0)crystals by the cooling of a saturate? solution which enters
t e crystallizer a t 120°F. The slurry leaving the crystallizer e l l be a t 80°F. Solu-
bility data are given in Fig. 11-9. Cooling water enters the crystallizer jacket a t 60°F
and leaves a t 70'3'. It may be assumed that the over-all coefficient of heat transfer for
t-stglljzer is 35 Bh/(hr)(sq ft)('F). There are 3.5 sq ft of cooling surface per foot
'
of crystallizer lenqt~~.
(a) ~stimate.thecooling wabr required in gpm.
(b) Determine the number of crystallizer sections to be used. \

Solutirm: Tnc yield may be calculated from the solubility data (see curve D, Fig.
11-9). At ~ J O O Fthe, saturated solution contains 140 parts of copperas per 1)(! parts
of excess ~ a t e r and
, the ssturated solution a t 80°F contains 74 >arts of oopperns per
. 100 parts of txcess water. The yitld will tilerefore be 66 ~ a a p e d P .p+rts
0 of e%cc$
' PC.

orater, o r S ~ a r $per 240 .parts of initial soluti~ri. The total a m o o f o n

. required is . &p*'
. .
(2000)(24?46).= 7270 lb/hr ' 0 .
4 .. . \

The. emling requirement m~,ynow be c a l c u l a ~ dby the procedure outlined, being th:
following data: , ,\
,i
\.'

Average specific heat of initial solution s'0.70 Btu/(lb)("F)

,
I
Heat of solution of PeSO4-7HzO a t 18°C = -4400 cal/g formula weight *
Based on the !zsr.~mptionsmentioned, heat of crpstallization of F e s o ~ . ' ~ ~-s O
-(-4400)(1.$ / X d = 28.5 :3tu/lb. It will be assumed that this value may be also
used at 80°F. Therefore, tb.? energy balance is

q = (72/0)(0.'70)(120.-- 80) + (20Wj(28.5) = 203,500 + 57,9OC =- 269,500 Btu/hr

3 .
The cooling water rzquirzd is.

i
Perry, p. 1052.
FIG.11.-9. Solubility of ferrous sulfete. Curves A, an and C as usually plitted; curve D
plotted as parts hydrate per 100 parts excess water.

The hmount of surface required is calculated from Eq. (4-41)

q = U A At,,,
60
All=120-70=50 Atz=80-60~20

At,,, =
50 - 20 = - 30
= 32.S°F
L
In ( 5 9 4 0 ) 0.916

Each 10-ft. section h s 35 sq ft of surfacc. Therefore, use seven sections.