3 DESIGNING OF CRYSTALLIZER

Crystallizers are used in industry to achieve liquid-solid separation. They are an important piece
of chemical processing equipment because they are capable of generating high purity products
with a relatively low energy input.

6.3.1Types of Crystallizer
 Forced Circulation
 Draft Tube Baffle
 Surface Cooled
 Batch Vacuum
 Scraped Surface

6.3.2 Selection of Crystallizer

We selected Scraped surface crystallizer on the following basis;

 Smaller equipment, which generally means less expensive installations, less floor space
needed, less operator labor.

 Better process control, fewer processes upsets.

 Extremely wide operating temperature range (-75C to +100C).

 Can be used at high process fluid viscosity.

 Simple, self-contained construction with minimal instrumentation and auxiliary

equipment.
6.3.3 Design of Crystallizer

Entering Stream Leaving stream

Crystallizer

Entering Stream

Component Weight entering(kg) Molecular weight Mass fraction

PTA 42045.45 166 0.246
Water 9127.79 18 0.0535
Acetic Acid 118823.139 60 0.6972
Impurities 420.45 150 0.00246
Total 170416.829

Leaving stream

PTA crystals 42045.45 166 0.246

Water 9127.79 18 0.0535
Impurities 420.45 150 0.00246

6.3.4 Crystal Growth Rate

Residence time in Crystallizer = t =30 min=1800 sec.

Length of Crystals = 125-135*10-6 m
Average length of crystals = 130*10-6 m
Lm=3.67G [23]
G=Lm/3.67
G=130*106/3.67(1800)
G=1.967*10-8 m/sec

So, Crystal growth rate = CGR= 1.967*10-8m/sec

6.3.5 Evaluation of Rate Constant

G=30/αKrρcLm4 [24]

α=shape factor (0.5 for PTA)

Kr=rate constant
ρc=density of crystals (1590 kg/m3)
Lm=length of crystasl (130*10-6m)

G=30/αKrρcLm4

Kr=30/α G ρcLm4

Kr=6.717*1021

6.3.6 Magma Density

In industrial crystallization, from solution the two phase mixture of mother liquor and crystals of
all sizes. In this case magma consist of

 Water
 Impurities
 PTA
 Acetic Acid
 Magma density can be determined by

ρm={(ρacetic acid*mass fraction A.A)+( ρPTA*xPTA)+( ρimpurities*ximpurities)}

ρm=1179.4552 kg/m3
6.3.7 Volume of Crystallizer

Qm=Mass flow rate/ρm

Qm=Volumetric flow rate
ρm=magma density
Total mass flow rate=170416.829kg/hr.
Magma density = ρm=1179.4552 kg/m3

Qm= 144.487 m3/hr

Volume of Crystallizer = V=Qm* t

V=144.487m3/hr *0.5 hr
V=72.24 m3

Safety allowance = 10%

Actual Volume =1.10*72.24
=79.64 m3

6.3.8 Dimensions of Crystallizer

Volume of the cylindrical tank = V= (3.14/4)*Dt2.H

Where,
Diameter of tank =Height of magma
Dt=H
So we can write,
V=(3.14/4)Dt3
Dt=(4/3.14*V)1/3
Dt=4.5 m
Diameter of tank = Height of magma

H=Dt=4.5 m
We know that
V=(3.14/4)Dt2.L
L=4V/3.14Dt2
L=4.9 m
6.3.9 Agitator design

1- Da/Dt=1/3

Da=dia of impeller = Dt/3=4.5/3 = 1.5 m

2- H/Dt=1/3

H=height of impeller

H=1.5 m

3- J/Dt=1/12

Baffle width = J = Dt/12

J= 0.376 m

4- L/Da=1/4

Length of turbine blade = L=Da/4

L=0.367 m

5- W/Da=1/5

W= width of blade

W=0.3008 m
Power Requirement:

Tip speed = 115ft/min

=35.0524 m/min

Tip speed =π NDa

N=tip speed/ π Da

N=7.4421 min-1

N=0.124sec-1

We know that

Re=Da2N ρm/µ

Re=9.92*105

If Re>104 then,
Np=Kt

P=Ktn3Da5ρ (Kt=5.75, McCabe and Smith table 9.2)

P=73.521 watt

P=0.098hp
 Since efficiency of motor is 85 % (from Perry’s hand book)

P=0.1/0.85
P=0.11 hp

6.4 Designing of cooling jacket (Around Crystallizer)

Heat balance:

Heat lost in solution = heat removed by cooling

Since, heat lost in solution = sensible heat + heat of crystallization

Sensible heat = mCp∆T

Q=[(mcp)CTA+ (mcp)water +(mcp)A.A+(mcp)p-xylene+(mcp)catalyst](110-45)

Qs=22.42*106kg/hr

Heat of crystallization = -15,500KJ/kmole

=-93.29 KJ/kg * 42045.24 kg/hr

=3.29*106kJ/hr

Heat lost in solution=22.42*106+3.92*106

=26.34*106kJ/hr

Heat lost in solution= heat removed by cooling

Heat removed by cooling = 26.34*106kJ/hr

6.4.1 Cooling jacket heat balance

Q=wcp∆T (T1=200C, T2=400C)

W=Q/ wcp∆T

W=315072 kg/hr
W=87.52 kg/sec

LMTD

110

45

40

20

LMTD= 43.700C

6.4.2 Outside film co-efficient

Working fluid is at 200C, for equivalent diameter of annulus, first find the other diameter of
cooling jacket. Velocity of water in annulus ranges from 0.3-1 m/sec (RC Vol 6.pg# 642)

U=0.3m/sec
ρ=1000 kg/m3

D1=(4.5+0.015) (4.5 is the diameter of crystallizer)

D1=4.515 m

D2=[(4W/ƛµ ρ)+d12]

D2=15.486 m

Equivalent dia. of annulus = De=D22-D12/D1

=De=48.623 m

Flow Area= Aa=π (D22-D12)/4

=172.10 m2

Mass Velocity = Ga=W/Aa

=0.508 kg/sec.m2

µ of water (at Tavg)=0.5064 *10-3 kg/sec.m

=1.82 kg/m.hr

Re. No. in annulus= GaDe/ µ

Re.No. = 48776.62

From graph the least L/D ratio.

Heat transfer factor= jH=4.2*10-3

=kwater=2.11 kJ/hr.m.0C

Pr.Np= cp µ/k

Pr.No= 3.60

Now, h0=jHRe(Pr)1/3*k/De

h0=13.56 W/m.sec

6.4.3 Inside film co-efficient

“CHILTON” gave the following empirical relation for jacketed vessel with agitator
(hi.D/k)=0.36(d2Ne/ µ)2/3(Cp µ/k)1/3(µ/ µw)0.24 (Perry’s handbook. Pg # 3-206)

hi=928.12 W/m0C

6.4.4 Overall heat transfer co-efficient

1/U0=1/h0+1/hod+d0ln(d0/di)/2kw+d0/di*1/hid+d0/di*1/hid+do/di*1/hi

hid=inside dirt co-efficient

hod=outside dirt co-efficient

outside dirt co-efficient = 4500 w/m2 0C (avg)

inside dirt co-efficient = 500 w/m2 0C

Thermal conductivity of wall = kw=16.27 w/m2 0C

By putting the values in above equation, we get,

Uo=10.59kj/hr.m0C

6.4.5 Heat transfer area Required

Q=UoA∆Tlm

A=Q/Uo∆Tlm
A=56.91 m2
Specification Sheet

Length of Crystals 130*10-6 m

Crystal growth rate 1.967*10-8m/sec

Magma Density 1179.4552 kg/m3

Volume of Crystallizer 79.64 m3

Diameter 4.5 m

Length of Crystallizer 4.9 m

0.11 hp
Power Required for Agitator

Cooling Jacket
LMTD 43.700C

Outside film co-efficient

13.56 W/m.sec

Inside film co-efficient 928.12 W/m0C

Overall heat transfer co-efficient 10.59 kj/hr.m0C

Heat transfer area required 56.91 m2

 6.5 Designing of Centrifuge
A centrifuge is most often used for the separation of particles from solutions according to their
size, shape, density, viscosity of the medium and rotor speed. These machines utilize the
natural separation realities present in a high-speed circular G-force environment.

6.5.1 Selection of Centrifuge

There are following factors which must be considered in the selection of centrifuge for a
process

 Current or past experience

 Physical Properties of Materials
 Specific Gravities of the Solids and Liquids
 Particle Size
 Performance Criteria
 Centrate Clarity
 Solid Recovery
 Solid Dryness
 Wash Efficiency
 Process requirements
 Pressure and Temperature
 Flow Rate (solid loading)
 Solid Concentration

So we selected Scroll Conveyor & Bowl Centrifuge.

6.5.2 Scroll Conveyor & Bowl Centrifuges

The Scroll Conveyor & bowl centrifuge is a continuous, sedimentation type unit comprising of
three primary components: a cylinder, conical bowl; a conveyer (e.g. a screw); and a gear unit
that provides the differential speed between the bowl and the conveyer. The centrifuge bowl
rotates clockwise at the speed required to generate the centrifugal force needed to effect the
intended separation. Slurry enters the centrifuge via a stationary pipe that empties into the hub
of the conveyer. In the hub, the feed is accelerated to the speed of the bowl and is fed through
an opening in the hub onto the inside surface of the bowl. The slurry quickly fills the bowl to a
height determined by the weir settings located at the larger-diameter end of the bowl.

Now Feed rate entering the Centrifuge is “F1”

F1= 170440.482 Kg/hr

Where F1 contains

Acidic Acid = 118823.139Kg/hr

CTA Crystals +Imp = 42045.4 Kg/hr

CTA Crystals +Imp = 42045.4 Kg/hr

H2O = 9127.79 Kg/hr

Catalyst = 259.6 kg/hr

 p - Xylene =184.51 Kg/hr

Filtrate leaving the Centrifuge is “F2”

F2=122069.299Kg/hr

Solid Feed rate leaving the Centrifuge is “F3”

F3=48496.58 Kg/hr

Where F3 contains

H2O = 6325 Kg/hr

CTA Crystals+Imp= 42171.586 kg/hr

6.5.3 Design Considerations

General design considerations for Scroll & Bowl Centrifuge are:

1. Volumetric flow rate entering

2. Length of centrifuge
3. Volume Of Bowl
4. Residence Time
5. Relative centrifugal Force
6. Settling Velocity Of Particles

6.5.4 Volumetric flow rate entering (Q)

Volumetric flow rate = Mass flow rate / Average density

To calculate the average density, we have data from “physioprops (software)”

 (At 45 C0 & 1 Atmosphere), Densities are as follows

Density of CTA = 1590 Kg/m3

Density of H2O = 989.672 Kg/ m3

Density of 4-CBA = 1021.95 Kg/ m3

Density of P- Xylene = 839.764 Kg/ m3

Average density calculated on basis of wt. fraction is given as

Avg Density = 989.672 *0.053 + 1590*0.246 + 839.764 * 0.001 + 1021.959*0.69

Avg density =1149.5 Kg/ m3

So from Eq. no. 1,

Volumetric flow rate = 170440.482/1149.5

Q = 148.26 m3 /hr

6.5.5 Length of centrifuge (L)

The ratio of L/D = 1.9 [25]

Diameter range = 100mm – 1400mm [26]

Diameter = D1 = 1400mm = 1.4 m

So ,

We know that, L/D = 1.9

Put the value of diameter in upper equation and get the length of centrifuge

L/1.4 = 1.9

L = 1.9 * 1.4

L = 2.66m

6.5.6 Volume of Bowl (V)

Volume of bowl is given below

V = * D2* L / 4

V = 3.1416*(1.4)2* 2.66 / 4

V = 4.06 m3

6.5.7 Residence Time (t)

Here Residence Time is

t = Volume of the liquid in the bowl / Volumetric Flow rate

Volume of liquid in the bowl is given below as

Where,
 L = 2.66m

D2 = 1.4 ; r2 = 1.4/2 = 0.7m

D1 = 0.8 ; r1 = 0.8/2 = 0.4m

Vl = * L* ( r22 - r12 ) (4)

Vl = 3.1416* 2.66* ( 0.72 - 0.42 )

Vl = 2.75 m3

So, t = 2.75 / 148.26

t = 0.018 hr

t = 1.11 min

6.5.8 Relative centrifugal Force

RPM of centrifuge = 1000 rev./min = 16.7 Hz (rev./sec) (5) & (6)

Here

RCF = Fc / Fg

RCF = 2 r / g

Where

 = Angular Velocity Of Bowl

 = 2 ** n

 = 2*3.1416*16.7

 = 104.9 Rad./ sec

 So

RCF = (104.9)2* 0.7 / 10

RCF = 770

6.5.9 Settling Velocity of Particles

We suppose laminar flow and consider that fluid is in stokes law range

that is Reynolds number is less than 1. For this situation settling velocity

is given below

Vs = Dp2 ( S – L ) 2 r2 /18  [27]

To calculate the average viscosity

Avg Viscosity = 5.87E-4*9127.19 + 8.45E-4*118823.13 + 4.82E-4*184.51/128135.439

Avg viscosity = 0.00082 pa.sec

Where

Dp= Minimum particle diameter = 130x10-6 m

 = Viscosity of liquid = 0.00082 Pa.sec

 = 104.9 Rad./ sec

r2 = 1.5/2 =0.7 m

Putting the values in above equation, we get

 Vs = (130*10-6)2 *(578.7)*(104 .9)2*(0.7) / 18* (0.00082)

Vs = 4.9 m/sec

Specification Sheet

Equipment Centrifuge

Function To Separate impurities

Operation Continuous

Type Scroll Conveyor & Bowl Centrifuge

Design Data
Flow rate of Solid entering 170440.482 Kg/hr
Outlet moisture content 0.15

Volumetric flow rate 148.26 m3 /hr

Diameter of Centrifuge 1.4 m

Length of Centrifuge 2.66 m

Volume of Bowl 4.06 m3

L/D ratio 1.9

Residence Time 1.11 Min

Settling velocity 4.9 m/sec