Technological Institute of the Philippines

CRYSTALLIZER
CR – 101
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SPECIFICATION SHEET

CRYSTALLIZER SPECIFICATION SHEET

TECHNICAL DATA
Type Vacuum Crystallizer
Material of Construction ASTM Type 304
Operating Temperature 10 oC
Operating Pressure 70 kPa
Volumetric Flowrate 73.1691 m3/hr
Residence Time 1.8832 hours
DESIGN DIMENSIONS
Volume 137.7897 m3
Diameter 4.8904 m
Height 7.3356 m
NOZZLE DESIGN
Nozzle Area 21.97 in2
Nozzle Inside Diameter 6.813 in
Nozzle Outside Diameter 8.625 in
Nozzle Thickness 0.906 in

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Stream 12
Composition Mass
NaCl(aq) 0.19
H2O(l) 18,750.77 Stream 13
NH4Cl(aq) 8,911.45 Composition Mass
NaHCO3 4.86 H2O(g) 208.06
NH4HCO3 0.14 Total 208.06
Total 27,667.40

Stream 14
Composition Mass
NaCl(aq) 0.19
H2O(l) 18,533.43
NH4Cl(s) 2,733.63
NH4Cl(aq) 6,174.73
NaHCO3 4.86
NH4HCO3 0.14
Total 27,446.98

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Supersaturation
From Particle Technology and Separation Processes, Vol. 2, 5 th edition. (Coulson and
Richardson).

∆c = c − c ∗
c
S=
c∗
∆c
∅= = S−1
c∗
Where:

c = solution concentration

c* = equilibrium saturation value

S = supersaturation ratio

∅ = relative supersaturation

Supersaturation can be generated depending on the solubility of the solute or more

𝑑𝑐∗
precisely on the slope of the solubility – temperature curve, .
𝑑𝑡

Solubility Curve of NH4Cl

90 y = 0.0012x2 + 0.3564x + 29.545
R² = 1
80
70
60
Solubility

50
40
30
20
10
0
0 20 40 60 80 100 120
Temperature

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Based from the solubility curve of the ammonium chloride, the slope generated is
2.0900.

S = 2.0900
c = 0.0099
Equilibrium Saturation Value
c
S=
c∗
0.0099
2.0900 =
c∗
c ∗= 0.0047

∆c = c − c ∗
∆c = 0.0099 − 0.0047

∆c = 0.0052
Relative Supersaturation
∆c
∅= = S−1
c∗
0.0052
∅= = 1.0900
0.0047
Population Balance, Nucleation, and Crystal Size
Assuming a MSMPR (Mixed Suspension, Mixed Product Removal)
crystallizer without agglomeration and breakage, operating at steady state (Myerson,
2002).

L
n′ = n°exp (− )
Gτ
Where:
n’ = number of crystals per unit size per unit volume of the system

n° = population density of the nuclei

LD = dominant crystal size
G = crystal growth rate

𝜏 = residence time

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According to a study, “Nucleation and growth rates of ammonium

chloride in organic media” (Randolph and Shadman, 1978), ammonium chloride
crystals precipitated in average size of 20 µm and dominant particle sizes of 50
µm. Therefore,
LD = 50 μm
L = 20 μm

According to PubChem, Open Chemistry Database, ammonium chloride

crystals are cubic in shape. Therefore,

K v = volume shape factor = 1

K s = surface shape factor = 6

Table 1. Kv and Ks Values for crystal shape

Geometric shape kv Ks
Sphere 0.524 3.142
Tetrahedron 0.118 1.732
Octahedron 0.471 3.464
Hexagonal prism 0.867 5.384
Cube 1 6
Needle 5 x 1 x 1 0.040 0.88
Needle 10 x 1 x 1 0.010 0.42
Plate 10 x 10 x 1 0.100 2.4
(Source: Crystallization Technology Handbook)

Acrystal = K s L2

Acrystal = (6)(2 × 10−5 )2

𝑨𝒄𝒓𝒚𝒔𝒕𝒂𝒍 = 𝟐. 𝟒 × 𝟏𝟎−𝟗 𝒎𝟐

Vcrystal = K v L3

Vcrystal = (1)(2 × 10−5 )3

𝐕𝐜𝐫𝐲𝐬𝐭𝐚𝐥 = 𝟖 × 𝟏𝟎−𝟏𝟓 𝐦𝟑

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𝐴𝑡
n° =
K s L2
2.4 × 10−9 (6)
n° =
6(3 × 10−3 )2
𝐜𝐫𝐲𝐬𝐭𝐚𝐥𝐬
𝐧° = 𝟎. 𝟗𝟔𝟎𝟎
𝐦 − 𝐦𝟑

L = 3Gτ (A.G. Jones, 200)

(5 × 10−5 ) = 3Gτ

Gτ = 1.6667 × 10−5 m
Substitute to the population balance equation,
L
n′ = n° exp (− )
Gτ
n′ L
= exp (− )
𝑛° Gτ
n′ 5 × 10−5
= exp (− )
𝑛° 1.6667 × 10−5

n′
= 4.9787 × 10−2 (4.9787%)
𝑛°
Thus 95.02129 % have been discharged by the time it reaches 50 μm.
Number of crystals/unit size/ unit volume:

n′
= 4.9787 × 10−2
𝑛°
n′
= 4.9787 × 10−2
crystals
0.9600
m − m3
crytals
n′ = 4.7796 × 10−2
m − m3

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Nucleation Rate
n°
B=
𝐺
B = k b ∆c b
G = kgS

Where
B = nucleation rate
G = growth rate
Kb = nucleation rate constant
Kg = growth rate constant
b = nucleation order
The nucleation rate constant for vacuum crystallizers with temperature profile
6.0920×10−8
ranging from 10°C to 40°C is , and nucleation order is 2.4930. (Molenaar,
𝑚3 −𝑚𝑖𝑛

2011).

B = k b ∆c b

6.0920 × 10−8 1min

B=( )( ) (0.0047)2.4930
𝑚3 − 𝑚𝑖𝑛 60s
crystals
B = 2.0180 × 10−15
m3 − s

(0.9600)(8 × 10−15 )(0.00002)

G=
(6.2479 × 10−11 )

G = 2.4584 × 10−9

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Gτ = 1 × 10−3

(2.4584 × 10−9 )τ = 1.6667 × 10−5

1.6667 × 10−5 1 ℎ𝑟
τ= −9 ×
2.4584 × 10 3600 𝑠𝑒𝑐𝑠
𝛕 = 𝟏. 𝟖𝟖𝟑𝟐 𝐡𝐨𝐮𝐫𝐬

Total Crystal Number (NT)

NT = n°Gτ
crystals
NT = (0.9600 ) (1.6667 × 10−5 m)
m − m3
𝐜𝐫𝐲𝐬𝐭𝐚𝐥𝐬
𝐍𝐓 = 𝟏. 𝟔𝟎𝟎𝟎 × 𝟏𝟎−𝟓
𝐦𝟑

Solids Production Rate

P = 𝜌𝑀 𝑄
Where
P = production rate

𝜌𝑀 = magma density
Q = volumetric flowrate

Magma density (from aspen) 1,134.3887 kg/m3

Total flowrate 27,667.40 kg/hr

𝑆ince the process is batch, the basis is 1 day of operation

kg 24ℎ𝑟𝑠 𝑑𝑎𝑦 3𝑠ℎ𝑖𝑓𝑡𝑠
𝑃 = 27,667.40 ( ) (1 )( )
hr 𝑑𝑎𝑦 1𝑠ℎ𝑖𝑓𝑡 24 ℎ𝑟𝑠
kg
𝑃 = 83,002.20
batch
P = 𝜌𝑀 𝑄
kg 𝑘𝑔
83,002.20 = (1,134.3887 3 ) 𝑄
hr 𝑚

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m3
Q = 73.1691
hr
Volume of the Crystallizer
𝑉 = 𝜏𝑄

m3
V = (1.8832 hours) (73.1691 )
hr

𝐕 = 𝟏𝟑𝟕. 𝟕𝟖𝟗𝟕 𝐦𝟑
Diameter of the Crystallizer
𝐻 3
= (𝑀. 𝐺𝑖𝑢𝑙𝑖𝑒𝑡𝑡𝑖 𝑒𝑡. 𝑎𝑙. ,2001)
𝐷 2

3 8𝑉
𝐷=√
3𝜋

3 8(137.7897)
𝐷=√
3𝜋

𝑫 = 𝟒. 𝟖𝟗𝟎𝟒 𝐦
Height of the Crystallizer
3
H = D( )
2
3
H = (4.8904 m) ( )
2
𝐇 = 𝟕. 𝟑𝟑𝟓𝟔 𝐦

Working Pressure
(3.5 atm)(101325 Pa)
P=
(1 atm)
P = 354,637.5 Pa ≈ 354.6375 kPa
Design Pressure
Design Pressure = 1.10(working pressure)
Design Pressure = 1.10(354,637.5 Pa)

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𝐃𝐞𝐬𝐢𝐠𝐧 𝐏𝐫𝐞𝐬𝐬𝐮𝐫𝐞 = 𝟑𝟗𝟎, 𝟏𝟎𝟏. 𝟐 𝐏𝐚 ≈ 𝟑𝟗𝟎. 𝟏𝟎𝟏𝟐 𝐤𝐏𝐚

Shell Thickness
PD
tp = +C
2fJ − P
Where:
tp = thickness of the shell
P = internal pressure
D = internal diameter
f = allowable working stress for stainless steel 304 (165 N/mm2)
J = efficiency (0.7)
C = corrosion allowance (3.81 mm)
PD
tp = +C
2Se − P
1000 mm
(0.3901 kPa)(4.8904 m × )
tp = m + 3.81 mm
2(0.7)(165000) − (0.3901 kPa)
t p = 𝟑. 𝟖𝟏𝟎𝟎 𝐦𝐦 ≈ 𝟒 𝐦𝐦

Inlet and Outlet Nozzle

kg
Density = 1,134.3887
m3
kg
ρV 2 = 1000
ms 2
kg
1000
v=√ ms 2
kg
1,134.3887 3
m
m
v = 0.9389
s
kg
feed flow rate = 23.0562
s

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𝑘𝑔
m (23.0562 )
𝑠
A= =
ρv (1,134.3887 𝑘𝑔 𝑘𝑔
) (0.9389 )
𝑚3 𝑠

𝐀 = 𝟎. 𝟎𝟐𝟏𝟔 𝐦𝟐
Nozzle Inside Diameter

4A
D=√
π

4(0.0216 𝑚2 )
D=√
π

𝐃 = 𝟎. 𝟏𝟔𝟔𝟎 𝐦 ≈ 𝟏𝟔𝟔. 𝟎𝟏𝟗𝟏 𝐦𝐦

Wall thickness of nozzle

Using the same computation for shell thickness in solving thickness of nozzle:

Pi di
tno = +C
2Jf − Pi

N 1000 mm
(0.3901 2 ) ( 0.1660 𝑚 × m )
tno = mm + 3.81 mm
N N
2(0.70) (165 ) − (0.3901 )
mm2 mm2

𝐭 𝐧𝐨 = 𝟑. 𝟖𝟏𝟎𝟑 𝐦𝐦 ≈ 𝟒 𝐦𝐦

Nozzle outside diameter, do

do = di + tno

do = 166.0191 mm + 4 mm

𝐝𝐨 = 𝟏𝟔𝟗. 𝟖𝟐𝟗𝟒 𝐦𝐦 ≈ 𝟎. 𝟏𝟔𝟗𝟖 𝐦

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Table 1 Nominal Sizing for nozzle pipe

Nominal Pipe Size 8 in

Schedule Number 160
Inside Diameter 6.813 in
Outside Diameter 8.625 in
Wall thickness 0.906 in
Area 21.97 m2
Source: Perry’s Chemical Engineering Handbook, 8th Ed.

Fig. 1 Table 10-22 Properties of Steel Pipe

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