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In the lithium carbonate precipitation process, sodium carbonate (Na2CO3) is added to the

reactor. Lithium sulphate reacted with the excess sodium carbonates to produce lithium

carbonate precipitation and sodium sulphate as a by-product. This reaction have high yield

of production where the production can achieved up to 99.6% of lithium carbonate.

Throughout this chapter, the proposed design of reactor used will be discussed and choose.

For the lithium carbonate precipitation, many types of reactor can be used such as batch

reactor, semi-batch reactor and continues stirred tank reactor (CSTR). Besides, in this

design, the parameters such as material of construction, cost of materials, installation and

operation of the reactor will be observed. The best reactor will be chosen and chemical and

mechanical design will be taken into account.

In the plant, reactor is considered as the heart of plant which can control the production of

the product. Lithium carbonate precipitation reactor is the most important equipment in this

production plant as it efficiency determine the production rate of the plant. Thus, the

selection of the best reactor for the process is important. This process occurs in slurry phase

where solid-liquid are taken into consideration. Since this process is vital in the production

processes, the design should take into consideration towards the highest output efficiency,

effective production and highest yield production. The comparison between potential reactor

used in this process are summarized in the table below.

Type of Batch reactor Plug flow reactor Continuous stirred

reactor tank reactor

principle

Raw materials are added One or more fluid is Reactants and product

Applicatio Disadvant Advantag Working

reaction and the outputs of reactor through the tube added and withdrawn

Suitable for are

the process reaction that

out after Highly

or pipe. adaptable with

Reaction using Highly

during the adaptable

process.

es

required long reaction time high efficiency reactor. reactor for large scale

and has high conversion. Operated mostly in production and high

Only for small scale of Used of plug

horizontal. flowbereactor

Can used Design

efficiency is complex.

reactor.

ages

recommend for large scale production is considered assumed perfect

Commonly

production. used in dyes

Operated in Used in industries where

not economical. Utilize

mixing and suitable

reaction in

is

and pharmaceutical pressure and most chemical

n

into consideration and

In order to achieve the desired conversion, a proper design reactor with implementation of

safety standard design is vital. For the high efficiency precipitation of lithium carbonate to

achieved, efficient mixing of the lithium sulphate and sodium carbonate is essential to

promote instantaneous reaction and to avoid undesired degradation reaction. The selection

of the appropriate reactor that suits the design basis needs to take into consideration. For

the lithium carbonate precipitation process, a continuous stirred tank reactor (CSTR) is

chosen as the best type of reactor that suitable for the condition. CSTR is suitable for a large

scale production and compatible with a process that needs high conversion and yield.

The CSTR is mounted with an agitator blade to ensure effective mixing as this

process needs to be in complete mixing between the reactants. CSTR is chosen instead of

batch reactor because it promising a large scale of production. For batch reactor, usually is

used for a small production plant with production rate below 500 ton/year. It is not suitable to

use plug flow reactor as our plant raw materials consist of slurry and solid material. The

CSTR is chosen as the design reactor in this plant. Figure below illustrate the configuration

of normal continuous stirred tank reactor (CSTR).

Figure: Continuous Stirred Tank Reactor

In lithium carbonate precipitation process, Sodium Carbonate will be added to the CSTR and

reacted with lithium sulphate and producing precipitate lithium carbonate and sodium

sulphate as a by-product. Chemical design is done to determine all possible reaction that

may occur in the reactor. In order to proceed with the chemical design, several assumptions

have been made which are:

2. The reaction is irreversible

3. The reactor is mounted with agitator to provide perfect mixing

4. The volume of reactor is constant throughout the process

5. No temperature gradient in the reactor (isothermal)

6. The density of material is constant throughout the process

7. The conversion is 99%

Chemical Reaction

In lithium carbonate precipitation process, sodium carbonate was added to the CSTR reactor

and contacted with lithium sulphate from the stream. The effluent of this process is lithium

carbonate which is the main product and sodium sulphate as the by-product of the process.

The chemical reaction involves in the process is as follows:

Where,

Data Extraction

The data from mass balance and summarize flow entering the Reactor; R-104 is

represented in figure. The table summarize the reactor condition.

F31 =

XH2O =

F34 =

XLi2SO4 =

FH2O =

XCaSO4=

XNa2SO4 = FCaSO4=

FCaCO3 =

F33 =

FNa2CO3 =

XNa2CO3 FNa2SO4 =

FLi2CO3 =

F31 F33 F34

Phase Slurry Solid Slurry

Temperature (oC) 95 oC 95 oC 95 oC

Pressure (bar) 3.447 3.447 3.447

Molar Flow 722.1309 36.80

(kgmol/hr)

Mass Flow (kg/hr) 18001.767 3900 21901.64

Density mix (kg/m3)

Determination of Concentration

By assuming that this reaction follows an elementary rate law, whereas the reaction orders

are identical with the stoichiometric coefficient of the reacting species for the reaction. The

rate law of the reaction can be written as:

m3

Where k is the rate constant for the reaction with unit ( )

mol . s

To determine the concentration of each species in the reaction, a stoichiometric

relationship between the reacting molecules for the reaction is established and tabulated in

table below.

Where: Li2SO4 = A

Na2CO3 = B

Li2CO3 = C

Na2SO4 = D

A FA0 -FA0X FA=FA0 - FA0X CA=CA0(1-X)

FA=FA0(1-X)

B FB0 -FA0X FB=FB0 FA0X CB=CA0(B-X)

FB=FA0(B-X)

C FC0 +FA0X FC=FA0X CC=CA0X

D FD0 +FA0X FD=FA0X CD=CA0X

CB0 FB0

B = =

C A0 FA 0

CB0 FB0

B = =

C A0 FA 0

B =

36.3793 kmol /hr

B =1.011

FA0 = CA0v0

The average volumetric flow rate of the system is vo = 3.337 m3/hr. Thus,

FA 0

C A 0=

v0

kmol 1 hr 1000 g

C A 0=36.3793 x x

hr 3.337 m 3

1 kg

mol

C A 0=10901.798

m3

C A =C A 0 (1 X )

mol

C A =10901.798 (10.99)

m3

mol

C A =109.02

m3

C B=C A 0 ( BX )

mol

C B=10901.798 3

(1.0110.99)

m

mol

C B=228.94

m3

CC =C A 0 X

mol

CC =10901.798 3

(0.99)

m

mol

CC =10792.78 3

m

C D =C A 0 X

mol

C D =10901.798 3

(0.996)

m

mol

C D =10792.78

m3

FA 0 X

V=

r A

C A 0 v0 X

V=

k CA CB

V X

=

v k C A 0 (1 X )( B X )

X

=

k C A 0 (1X )(B X )

X

k=

C A 0 (1X )(B X )

0.99

k=

3600 s mol

2 hr x x 10901.798 3 (10.99)(1.0110.99)

1hr m

3

m

k =6.006 x 105

mol . s

C

[ B]

CA

r A =k

5 m3 mol mol

r A =6.006 x 10 x 109.02 3 x 228.94 3

mol . s m m

mol

r A =1.50 3

m .s

r A =1.50 x x

m . s 1000 mol 1 hr

3

kmol

r A =5.4292

m3 . h

According to the definition of CSTR, the steady state mixed reactor equation is as below:

Thus:

F A 0F A

V=

r A

FA 0 X

V=

r A

kmol

36.3793 x 0.99

hr

V=

kmol

5.4292 3

m . hr

3

V =6.67 m

The reactor diameter and height of CSTR reactor can be calculated using some

assumptions:

2. Fully mixing

3. Ratio of all equipment measurement is 0.5 an diameter of vessel is equal to height of

liquid

Volume of CSTR

DT2

V = xH

4

From equation

DT H

=

D D

D T =H

DT H

= D T =H

D D

Therefore,

DT3

V = =6.67 m3

4

4(6.67)

DT =

3

3

D T = 8.4925

D T =2.05 m

D T 2.1 m

Using safety factor of 10% for the height of the reactor to avoid the overflow and overheated

in the reactor. The height of the reactor can be calculated as below:

In the mechanical part, in order to design the CSTR reactor, a few parameters that take part

in the design are:

2. Material of construction (MOC)

3. Equipment dimension

4. Other important part

The material of construction selected for this design is stainless steel 316 because of its

ability to withstand corrosive materials. Sodium Carbonate is one of material with strong

base properties and the reaction can be corrosive in nature. In chemical industry, stainless

steel is usually used form construction of equipment to counter the corrosive reaction or

materials. Selection of material must take into account the suitability of the material for

fabrication especially welding and also the compatibility of the material with process

environment.

Joint efficiency is a factor included into the formula for calculating the vessel wall thickness.

The welding efficiency for the reactor design is selected to ensure the strength of the weld.

According to the book Chemical Engineering Design, the joint factor used in each design will

depends on the type of joint and amount of radiography required by the design code. The

typical values for maximum allowable joint efficiency are shown in the table (Sinnott, 2005).

Taking the factor as 1.0 for this design implies that the joint is equally as strong as the virgin

plate or fully radiographed.

Figure: Maximum allowable joint efficiency (Sinnott, 2005)

Corrosion Allowance

Other important criteria need to be considered in this design is the corrosion allowance. By

knowing the unexpected general corrosion rate and the anticipated plant or service life of a

part, we can calculate the extra thickness required for the design to resist corrosion from the

process. Corrosion allowance is added to the wall thickness to compensate for the metal

expected to be lost over the life of the equipment. The MOC chosen is stainless steel 316

has the best corrosive resistance. According to the ASME BPV Code, minimum corrosion

allowance chosen for this CSTR design is 4mm which is believe to be adequate to withstand

the corrosion problem for the reactor.

Design pressure

The operating pressure of the reactor is 3.447 bar which is 344.7kPa gauge. By taking the

design pressure 10% above operating pressure:

N

mm2

PDesign =1.1 x 3.447 x 0.1

Design Temperature

The design temperature is equal to the operating temperature of the reactor:

T Design =95 oC

As reference to British Standard, PD 5500, the nominal strength which is also called

allowable design stress are listed in the standard for the range of material covered by the

standard. The typical design stress values for some common material are shown in table

below. By using interpolation methods, the design stress for this design is calculated.

10095 145 X N

= X =147 2

10050 145165 mm

Therefore, the design stress for this CSTR reactor that operates at 95oC is 147 N/mm2

Metal Thickness

To ensure that the vessel is sufficiently rigid to withstand its own weight and any accident

load, the minimum wall thickness is calculated. For CSTR, a cylindrical shell, the minimum

thickness required to resist internal pressure can be determined by:

Pi D i

e=

2 f Pi

Where,

e Minimum thickness, mm

Di Internal diameter, mm

e= e=2.72 mm

2 (147 )0.38

With the addition of 4mm corrosion allowance, the required metal thickness therefore,

e=2.72 mm+4 mm

e=6.72 mm

In design of top and bottom and cover head, there are many type of with various shape that

is commonly used for the reactor. The common type used is:

Hemispherical

Ellipsoidal head

Tori spherical

Figure: Types of dooms head (a) Hemispherical (b) Ellipsoidal (c) Torispherical

t=D e

CPi

SE

Where,

t=1.7 x 103

0.25 x 0.38

147 x 1.0

t=43.22 mm

Adding the corrosion allowance of 4mm, therefore

t design=47.22mm

t= t= t=1.36 mm

4 SE0.4 Pi 4 ( 147 ) ( 1 )0.4 ( 0.38 )

t design=5.36 mm

P i Di 0.38 x ( 2.1 x 10 3)

t= t= t=2.71 mm

2 SE0.2 Pi 2 ( 147 ) ( 1 )0.2 ( 0.38 )

t design=6.71 mm

t= t= t=4.81 mm

SE0.1 Pi ( 147 ) ( 1 )0.1 ( 0.38 )

t design=8.81 mm

Table: Summary table for Metal Thickness Calculation for different design.

Flat Head 47.22 mm

Hemispherical Head 5.36 mm

Ellipsoidal Head 6.71 mm

Torispherical Head 8.81 mm

Based on table, the ellipsoidal design cover calculation shows the metal thickness that about

the same with the body thickness 6.71 mm. For this design, ellipsoidal head cover is

Figure: Major and Minor axis of ellipsoidal (a) Major axis, R=2r (b) minor axis = r

From the figure, major axis is equal to the internal diameter of the cylinder which is 2.1m.

2.1

2 R=2.1 m R= =1.05 m

2

For the minor axis, the radius, r can be calculated by using formula:

1.05

R=2 r 2 r=1.05 m r= =0.525 m

2

The height of the dome is equal to the radius of minor axis, so:

H , ( h )=0.53 m

Agitator Design

Process of precipitation of Lithium carbonate need a proper mixing between Lithium Sulfate

and Sodium Carbonate in the reactor. The type of agitator used with the reactor will be

chosen based on type of mixing required, fluid properties, viscosity of the reactant and

capacity of the vessel.

For this design, pitch blade impeller is chosen for the reactor. Pitch blade using axial

flow pattern which it can solve two challenges of mixing; solid suspension and stratification.

Exceptional top to bottom motion in tank is providing especially when it is placed over the

center of a baffled vessel. Besides, the superficial and annular velocities can be altered to

adjust the mixing levels. Pitched blade impellers, which are known for the versatility and

ability to create a balance of flow and shear. Pitched blade impellers are particularly useful

when mixing viscous fluids with a lower bottom clearance as well as a shallower submersion.

Figure show the configuration of pitch blade impeller with axial flow turbine type. It is

using 4 blade and for mixing of medium viscosity material, it is more economical than 3

blades impeller. Material used for the impeller is the same as the reactor materials which is

stainless steel to avoid the corrosion problem inside the reactor.

Figure: Pitch Blade Turbines

The distance of the blade and bottom of reactor is assumed to be a one third of the reactor

diameter,

2.1 m

Eb = Eb =0.7 m

3

The design of the blade is calculated based on assumption; the length of the blade is one

third of the reactor diameter:

2.1 m

Lb = Lb=0.7 m

3

0.7 m

W b= W b =0.2333 m

3

Shaft Design

Shaft is a crucial part of agitator as the function of shaft is to transmit the torque from the

drive train to the impeller in the reactor. In designing shaft, the design must accommodate

hydraulic and mechanical loads and vibration near the natural frequency must be avoided. In

order to avoid problems during the operation of the reactor, the design of the shaft must

have sufficient structural strength and allowed for the bending moment to withstand the

hydraulic force acting on the impellers in the reactor. A proper design of shaft is needed in

order to avoid any disturbance during the process of the reactor.

Agitator Power

H p= pV

Where

Hp Agitator power

V Volume of reactor, m3

Typical power consumption per volume is given as 0.2kW/m 3 foe medium viscosity

(Sinnott, 2005). Therefore using the equation above, the power of agitator can be calculated

as:

kW

H p=(0.6 3

) x 6.67 m3

m

H p=4.002 kW H p=5.37 hp

The torque transmitted by the shaft will have the maximum value above the uppermost

turbine. Since the power drawn by sealing devices is in significant, the calculation torque is

as below:

Hp

T Q (max )=63025

N

Whereas,

5.37 N

T Q (max )=63025 x T Q (max )=2820

120 mm2

To calculate the maximum bending moment, the sum of the product of the hydraulic forces

and the distance from the individual impellers to the bottom bearing in the mixer drive is

defined. The equation below computes an empirical hydraulic force related to the impeller

torque acting as load at a distance related to the impeller diameter.

M m ax =19000 ( HNDL )

p

Where,

L Length of vessel

D Blade diameter

5.37 )( 2.31 ) N

M max=19000 (( 120 ( 0.7 ) ) M max=2805.83

mm2

The relationship to meet the shear stress and tensile stress can be used to calculate the

minimum shaft diameter values. Since the bending moment and the torque act

simultaneously, these loads must be combined and resolved into a combined shear stress

and combined tensile stress acting on the shaft. The minimum shaft diameter for the

allowable shear stress can be calculated as follows:

ds =[ 16 T 2Q (max ) + M 2max

s ] 3

For stainless steel 316, the recommended allowable shear stress and tensile stress is 6000

and 10,000 psi respectively. Therefore, shear stress diameter can be calculated as below:

ds =

[16 28202 +2805.832

( 6000 ) ] 3

d s =1.5 d s =3.81cm

]

2 2

max ) 3

dt =

t

dt =

[16(2805+ 28202 +2805.832)

( 10000 ) ] 3

d t =1.5117 d t =3.84 cm

Therefore, to meet the shear and tensile stress requirement, a 3.9 cm of shaft

diameter is recommended for this design.

The weight of impeller can be varied based on the manufacturer. The following calculation is

only to determine the approximate weight of impeller. Table below shows the standard hub

weight that available in the industries. The weight will then be added to the weight calculated

in the equation.

Based on the table, the weight of the hub is estimated to be 5kg as the shaft diameter is 3.9

cm. Therefore, to calculate the individual impeller, the following equation is used:

1

0.35 D3 H p

W b= ( N )

2

Where

Wb Weight of Blade

Hp Agitator Power

N Speed Impeller

1

0.35 ( 0.7 )3 (5.37)

W b= ( 120 ) 2

W b =0.0733 kg

wL

W e =W +

4

Where,

w Shaft diameter

L length of shaft

Length of shaft = height of reactor distance between bottom reactor and impeller)

0.039 ( 2.310.7 )

W e =4 ( 5.1 ) + W e =20.4 kg

4

6 2

0.388 x 10 ( d Fm )

N c=

L W s L+ Sb

Where,

d Diameter shaft, mm

Ws Equivalent weight

Sb Bearing span

L = 1610mm

6 2

0.388 x 10 ( 39 x 1 )

N c=

1610 20 1610+0.35

N c =2042.49 rpm

The operating speed assume for this design is 120 rpm, since the natural frequency

analysis calculated is more than the operating speed, the 3.9cm shaft is acceptable for this

reactor design.

Baffles Design

Baffles are flow directing or obstructing vanes or panels used in vessels (tanks), for this case

is in CSTR reactor. Baffles are design to support tube bundles and direct the flow of fluids for

maximum efficiency. In chemical reactor, baffles are often attached to the interiors walls to

promote mixing and thus it will increase the heat transfer and possibly chemical reaction

rates. Baffle design is one of important criteria to ensure there is adequate baffling for good

mixing by providing a flow pattern throughout the entire vessel. Baffles also installed in

reactor to avoid excess swirling and vortexing, assure a stable and consistent power draw

and produce more uniform radial shaft load.

This reactor is equipped with four baffles with one tenth of the tank diameter in width as

illustrated in the figure above. Baffle width can be calculated using formula:

1 1

W b= x Di W b= x 2.1 W b =0.21 m

10 10

This reactor is assumed to be isothermal reactor which means there is no heat in or out of

the reactor during the process. Jacketed vessel is a container that is designed for controlling

the temperature of its contents. By using the cooling or heating jacket around the vessel

through which a cooling or heating fluid is circulated. For this design of CSTR, an external

jacket is chosen to be the heat transfer medium instead of coil as the process involving a

chemical with high base which have high potential of corrosion.

There are several types of jacket in industries, which are conventional jackets, half

pipe coils jacket, dimple jackets and plate coils. Conventional jacket is usually in reactor

jacket design. A second shell is installed over a portion of the vessel, creating an annular

space within which cooling or heating medium flows. A simple conventional jacket, with no

internal components, is generally very inefficient for heat transfer because the flow media

has an extremely low velocity resulting in a low heat transfer coefficient.

The heating medium used in this design is hot water inlet temperature of T j,0 =100oC. the

operating temperature of the reactor is maintained at 95 oC throughout the process. The

heating jacket is design to replace the heat loss caused by heat of reaction during the

process. The heat added by the reactor is Q = 179008.96 W. the properties of hot water at

100oC is obtained from Improved international formulations for the viscosity and thermal

conductivity of water substance and tabulated in table.

Table: Physical Properties of Water at Tc,in=100oC

Viscosity, 281.8 Pa.s

Density, 958.4 Kg/m3

Thermal conductivity, 0.6791 W/m.K

K

Heat specific capacity, 4215.9 J/kg.K

Cp

The total heat added by the cooling water can be calculated using this equation:

hw =hw vA

Where,

Using velocity of 0.2m/s to estimate the heat transfer coefficient and the thickness of

the wall is 6.72 mm as calculated in previous section, the heating jacket thickness is

assumed to be 100mm to aid the calculation, the inlet and outlet diameter of jacket can be

determined.

Therefore,

D j0

2

( 2D j )

4

hw =hw v

2.3134

( 22.1134 2 )

kg

hw =133.29

s

4

hw =958.4 (0.2)

For design of isothermal reactor, the heat released from the reactor is equal to the heat

added by the heating medium. Therefore the relationship of these two can be defined as,

179008.96

T =

hw C p , hw

179008.96

T =

kg J T =0.3186 K

133.29 x 4215.9

s kg . K

Then the outlet temperature of the heating water leaving the jacket can be calculated as:

Next, the surface area for the heat transfer is calculated by using overall heat transfer

coefficient, U for the reaction. To calculate U, the following formula can be used,

1 1 dW 1

= + +

U h 0 K hi

Where,

hi Enthalpy of fluid mixture

Viscosity, 0.000350666 Pa.s

Density, 857.6077 Kg/m3

Thermal conductivity, 3.6420 W/m.K

K

Heat specific capacity, 2206.67 J/kg.K

Cp

h=C p T

1 1 dW 1

= + +

U Cp w T j K Cpmix T

1 1 0.00672 1

= + +

U (4215.9)(367.6814) 3.6420 (2206.67)(368)

Bibliography

Edward, C., Victor, A., & Suzzanne, M. (2004). Handbook of Industrial Mixing.

Scince.

Heinemann.

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