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CRYSTALLIZATION
Refers to a solid-liquid separation process in which solid particles are formed within a homogenous phase.
It can occur as:
I. formation of solid particles in a vapor
II. formation of solid particles from a liquid melt
III. formation of solid crystals from a solution
Crystal Geometry
A crystal is highly organized type of matter, the constituent particles of which are arranged in an
orderly and repetitive manner; they are arranged in orderly three-dimensional arrays called SPACE LATTICES.
Supersaturation
Supersaturation is a measure of the quantity of solids present in solution as compared to the quantity that is in
equilibrium with the solution.
Crystallization cannot occur without supersaturation. There are 5 basic methods of generating
supersaturation
a. EVAPORATION – by evaporating a portion of the solvent
b. COOLING – by cooling a solution through indirect heat exchange
c. VACUUM COOLING – by flashing of feed solution adiabatically to a lower temperature and inducing
crystallization by simultaneous cooling and evaporation of the solvent
d. REACTION – by chemical reaction with a third substance
e. SALTING – by the addition of a third component to change the solubility relationship
Crystallization Mechanism
There are two basic steps in the over-all process of crystallization from supersaturated solution:
NUCLEATION.
i. Homogenous or Primary Nucleation – occurs due to rapid local fluctuations on a molecular scale in a
homogenous phase; it occurs in the bulk of a fluid phase without the involvement of a solid-fluid interface
ii. Heterogeneous Nucleation – occurs in the presence of surfaces other than those of the crystals such as the
surfaces of walls of the pipe or container, impellers in mixing or foreign particles; this is dependent on the
intensity of agitation
iii. Secondary Nucleation – occurs due to the presence of crystals of the crystallizing species.
CRYSTAL GROWTH – a layer-by-layer process
a. Solute diffusion to the suspension-crystal interface
Classification of Crystallizer
i. May be classified according to whether they are batch or continuous in operation
ii. May be classified according on the methods used to bring about supersaturation
iii. Can also be classified according on the method of suspending the growing product cry
Forced circulation crystallizer (MSMPR Crystallizer)
Forced circulation crystallizer uses to get better crystal growth rate and to keep crystals in suspension throughout
the crystallization zone.
Process
In heat exchanger, feed slurry is firstly introduced.
After that pumped to main body. At the top surface of slurry, vaporization takes place. Nucleation is done
close to the bottom of the body.
Crystals are then separated and removed.
Solvent, that is vaporized, is condensed and returned to the crystallizer body.
ADVANTAGES
Least expensive.
Gives large range of crystals.
Particle deposits on body walls are reduced due to high circulation rate.
DISADVANTAGES
Control of crystal size is difficult.
GROWTH RATE:
𝐸
𝐺 = 𝑘𝑔 × 𝑒 𝑅𝑇 × 𝑆 𝑔 i
Where
G=Growth rate
𝑘𝑔 =Growth rate constant
E=activation energy of growth rate
S=Supersaturation
𝑗
T=314 K R=8314 𝑘𝑚𝑜𝑙.𝑘
𝑗 ii
E=10400 𝑘𝑚𝑜𝑙
……………………………. Page 1621(1)
𝐶 ° −𝐶 iii
𝑆= 𝐶°
Calculating 𝐶 ∗
𝑙𝑜𝑔𝐶 ∗ = 𝛼𝑇 + 𝛽iv………………………page 235(2)
Put values in equation:
𝑙𝑜𝑔𝐶 ∗ = [(2.25 × 10−2 ) × (314)] + (−0.424)
𝑔
𝑙𝑜𝑔𝐶 ∗ = 6.641 𝑔 𝑓𝑟𝑒𝑒 𝑝ℎ𝑒𝑛𝑜𝑙
Calculating C
1 1
𝐶 = 𝐾𝐶 𝑆 𝑚 (𝑢3 + 𝑣 3 )3 ………………………. page 235(2)
v
Where
u = crystal size
v=particle size actual
so 𝐾𝐶 𝑖𝑠 𝑧𝑒𝑟𝑜 𝑑𝑢𝑒 𝑡𝑜
𝐾𝑐 = 0 , 𝐶 = 0vi
106.646
𝑆 = 106.646 = 1
−𝟏𝟎𝟒𝟎𝟎𝑬 𝒖𝒎
𝑮 = 𝟎. 𝟎𝟒𝟓 × 𝒆𝟖𝟑𝟏𝟒×𝟑𝟏𝟒 × 𝟏𝟏.𝟏𝟒 = 𝟎. 𝟎𝟒𝟒𝟑𝟑
𝒔
Nucleation Rate:
−𝐸
𝐵 = 𝐾𝑛 × 𝑒 𝑅𝑡 × 𝑆 𝑏 × 𝑀𝑡 1.17 vii…………………………page 1618(1)
Here
𝐾𝑛 =Nucleation Rate Constant
S =Supersaturation
𝑀𝑡 =Magma Density
Magma density:
𝑀𝑡 = 6 × 𝑘𝑣 × 𝜌𝑐 × 𝑛° × 𝜎 4
−𝟏𝟏𝟎𝟎𝟎 𝟏
𝑩 = 𝟑𝟗𝟖 × 𝒆𝟖𝟑𝟏𝟒×𝟑𝟏𝟒 × 𝟏𝟏.𝟏𝟒 × (𝟔 × 𝟏 × 𝟏𝟑𝟓𝟕 × × 𝟏𝟑𝟑. 𝟑𝟒 )𝟏.𝟏𝟕
𝟎. 𝟎𝟒𝟒𝟑
𝟏
= 𝟖. 𝟑𝟓 × 𝟏𝟎−𝟏𝟐
𝒌𝒈 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏. 𝒔
𝑀𝑡 = 6 × 𝑘𝑣 × 𝜌𝑐 × 𝑛° × 𝜎 4
𝟖. 𝟐𝟔 × 𝟏𝟎−𝟏𝟐 𝒌𝒈𝒄𝒓𝒚𝒔𝒕𝒂𝒍
𝑴𝒕 = 𝟔 × 𝟏 × 𝟏𝟑𝟓𝟕 × × 𝟏𝟑𝟑. 𝟑𝟒 = 𝟒𝟕𝟗. 𝟖 ≈ 𝟒𝟖𝟎
𝟎. 𝟎𝟒𝟒𝟑 𝒌𝒈𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏
Volume of Crystallizer
3 4𝑉
𝐷𝑖𝑎 𝑜𝑓 𝑉𝑒𝑠𝑠𝑒𝑙 = √ xiii
𝜋
3 4 × 3.486
𝐷𝑖𝑎 𝑜𝑓 𝑉𝑒𝑠𝑠𝑒𝑙 = √ = 1.65 𝑚
𝜋
𝐷 0.1 × 𝐷
𝐻𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐶𝑜𝑛𝑒 = 𝑡𝑎𝑛45( − )
2 2
1.65 0.1 × 1.65
𝐻𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐶𝑜𝑛𝑒 = 𝑡𝑎𝑛55 ( − ) = 1.06 𝑚
2 2
3
𝐻𝑒𝑖𝑔ℎ𝑡 𝑡𝑜 𝐷𝑖𝑎 𝑟𝑎𝑡𝑖𝑜 𝑜𝑓 𝑐𝑦𝑙𝑖𝑛𝑑𝑟𝑖𝑐𝑎𝑙 𝑠𝑒𝑐𝑡𝑖𝑜𝑛 =
2
𝐻 3
= = 𝐻 = 1.5𝐷 = 2.475 𝑚
𝐷 2
Add 1.25 space above the Boiling for disengaged of Droplet:
𝐻 = 2.475 + 1.25 = 3.725 ≈ 3.75 𝑚
𝐷2
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐶𝑦𝑙𝑖𝑛𝑑𝑟𝑖𝑐𝑎𝑙 𝑠𝑒𝑐𝑡𝑖𝑜𝑛 = 𝑉𝑐 = 𝜋 × × 1.5 × 𝐷 = 5.289 𝑚3
4
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐶𝑜𝑛𝑖𝑐𝑎𝑙 𝑠𝑒𝑐𝑡𝑖𝑜𝑛 = 𝑉𝑐 = 0.2616 × 𝐷3 = 1.17 𝑚3
𝑻𝒐𝒕𝒂𝒍 𝑽𝒐𝒍𝒖𝒎𝒆 = 𝑽𝒕 = 𝟓. 𝟐𝟖𝟗 + 𝟏. 𝟏𝟕
= 𝟔. 𝟒𝟔 𝒎𝟑
Allowable velocity:
Using Souder-Brown Equation to determine the allowable Velocity of the Vapor without risking entrainment.
𝜌𝑙 − 𝜌𝑣
𝑈𝑣 = 𝐶𝑣 × ( )xiv
𝜌𝑣
𝑚
𝑊𝑖𝑡ℎ 𝐷𝑒𝑚𝑖𝑠𝑡𝑒𝑟 𝑝𝑎𝑑 𝐶𝑣 = 0.04
𝑠
1020 − 0.59 𝑚
𝑈𝑣 = 0.04 × ( ) = 1.66
0.59 𝑠
Area required for Evaporation:
𝑄 = 𝑈𝑣 × 𝐴
𝟏. 𝟎𝟏 × 𝟏𝟎𝟒
𝑨= = 𝟏. 𝟔𝟗 𝒎𝟐
𝟏. 𝟔𝟔 × 𝟑𝟔𝟎𝟎
𝑁
𝐷𝑖 = 1.65 𝑚 = 0.05
𝑚𝑚2
Formula for calculating Thickness of Shell:
𝑃𝑖 × 𝐷𝑖
𝑒=
2𝑓 − 𝑃𝑖
Where f is design stress taken from table in book:
𝑵
𝒇 = 𝟏𝟑𝟓
𝒎𝒎𝟐
𝑁
𝑃𝑖 = 0.50 𝑏𝑎𝑟 = 0.05
𝑚𝑚2
As 10 % above for pressure
𝑁
𝑃𝑖 = 0.50 𝑏𝑎𝑟 = 0.055
𝑚𝑚2
𝑁
𝑅𝑐 = 1.65 𝑚 = 0.05
𝑚𝑚2
Knuckle radius is 6% of R
𝑁
𝑅𝑘 = 1.65 × 0.06 𝑚 = 0.099
𝑚𝑚2
1 𝑅𝑐 1 1.65
𝐶= [3 + √ ] = [3 + √ ] = 1.78
4 𝑅𝑘 4 0.099
𝑃𝑖 × 𝑅𝑐 × 𝐶
𝑒=
2𝐽𝑓 + 𝑃𝑖 (𝐶 − 0.2)
J is taken by 1 there will be no joint in Head
0.055 × 1.77 × 1650
𝑒= = 0.54 𝑚𝑚
2 × 135 + 0.05(1.77 − 0.2)
𝑃𝑖 × 𝐷𝑖
𝑒=
2𝑓 − 0.2𝑃𝑖
Since our reaction is the gaseous phase and exothermic reaction so the choice is the tubular reactor.
Selection of the bed
Use of the catalyst requires modifications to basic reactor design to fixed bed reactors, moving bed reactors or fluidized bed
reactors.
Fixed bed reactors
These are used in the heterogeneous catalyst reactions and pressure drop across the bed is small. The design of the fixed bed
reactor is very easy as compared to the moving bed and fluidized bed reactors. Their size is also compact as compared to
other fluidized bed and moving bed reactors. The energy requirement is also small because no amount of energy is needed as
in fluidized bed and moving bed required to fluidize or move the bed.
Fluidized bed reactor
These are the reactors with a gas phase working fluid that requires gas flow around and across the fine particles at a rate
sufficient to fluidize the particles suspended within the reactor. Since the catalyst bed has to be fluidized so the energy
requirement in these reactors is large. Pressure drop is also large as compared to the fixed bed reactors because the pressure is
dissipated to fluidize the bed. The volume of the reactor required is also large as compared to fixed bed reactor, because the
void spaces between the fluidized beds occupy the more volume.
Safety factors:
The confinement of hazardous reactants and products, and the control of the reaction and the process conditions
DESIGN CALCULATION
The reaction occurring in Adiabatic Fixed Bed reactor is heterogeneous reaction, the reactants are in liquid phase and the
catalyst is in solid phase. The process is continuous. Since the Adiabatic Fixed Bed reaction is endothermic reaction so heat
will be not be generated.
Feed to reactor
stream inlet Molecular Kg/hr Kmol/hr Mol fraction
weight
PARAMETER EVALUATION
-
k=Aexp−Ea/RT
A=24600exp(-E/RT)
Ea=-20500 kcal/mol
R=8.314
T=343K
k=24600^exp(-20500/8.314*343)
(REF)
k=20.5
REACTION
ACETONE+PHENOL BISPHNOL+WATER
Rate of reaction on depends on the single reactant
CALCULATION OF CONCENTRATIONS
CAo CA=Cao(1-X) kmol/m3
CA1 (At 0% Conversion) 0.5 kmol/m3
CA2 (At 9.7% Conversion) 0.4515 kmol/m3
CA3 (At 19.4% Conversion) 0.403 kmol/m3
CA4 (At 29.1% Conversion) 0.3545 kmol/m3
CA5 (At 38.8% Conversion) 0.31 kmol/m3
CA6 (At 48.5% Conversion) 0.2575 kmol/m3
CA7 (At 58.2% Conversion) 0.209 kmol/m3
CA8 (At 67.92% Conversion) 0.1605 kmol/m3
CA9 (At 77.6% Conversion) 0.112 kmol/m3
CA10(At 87.3% Conversion) 0.0635 kmol/m3
CA11(At 97% Conversion) 0.015 Kmol/m3
At 97% conversion
Weight of catalyst is
XA dX A
W = FAo *
o -rA
where
X A dX
o -rAA = Area under the curve
Area under the curve is found by applying Trapezoidal rule
Applying trapezoidal rule,
-
0.97−0
= 𝑥 (1.673717+2(0.423532)+2(0.31779)+2(0.7602)+2(1.00482)+2(1.16995)+2(1.2473)+2(1.27906)+2(1.28153)+2(
2
1.26521)+ 1.23701)
VOLUME OF REACTOR
e= Thickness (m)
Pi= Internal Pressure (kPa)=1.1 x 410.325= 451.3575kPa
Di= Internal Diameter (m)=1.38m
THICKNESS FOR CYLINDERICAL 0.00560m 5.60 mm
SECTION (m)
CLOSURE SELECTION OF ELLIPSOIDAL HEAD
𝐏𝐢 𝐃𝐢
е= 𝟐𝐉𝐟−𝟎.𝟐𝐏𝐢
ɸ (POROSITY) 0.4
(Dp) DIAMETER OF
CATALYST PARTICLE 0.005 m
AVERAGE VISCOSITY OF
FEED 0.0000128442 kg / m.s
AVERAGE DENSITY OF
FEED 0.928 kg / m3
Mw (AVERAGE
MOLECULAR WEIGHT) 76 kg / kmol
PRESSURE DROP
(ΔP) 8112.25 Pa
PRESSURE DROP
Kpa
OR (ΔP) 8.1125
OR
The pressure drop is in appropriate range and within 10% of the Operational pressure
Specification Sheet
Reactor
ID number: R-100
Design data
Type Fixed Bed
Position Vertical
Material of construction Stainless steel
Weight of catalyst (kg) 4546.4
Diameter of Reactor (m) 1.38
Height of Reactor (m) 5.8
Volume of Reactor (m3) 6.18
Pressure Drop(kpa) 8.112
1. Green, D. (2008). Perry's chemical engineers' handbook. New York [etc.]: McGraw-Hill.
2. Edgar, T. (2008). Perry's chemical engineers' handbook. 1st ed. [New York]: McGraw-Hill.
3. Fogler, H. Scott. (1999). Elements of chemical reaction engineering. Upper Saddle River, N.J.
:Prentice Hall PTR,
Heat exchanger is an important equipment used in almost every chemical industry. A heat exchanger is an
effective equipment used for heat transfer from one medium to another. They were extensively used in
different in power plants and in both petrochemical and petroleum industry.
There are many configurations of heat exchangers available for different heat transfer operations. Heat
exchangers can be classified on the basis of their basic operation, flow arrangement and etc.
Tubular heat exchangers are made of circular tubes. Tubular heat exchanger are primarily used for liquid to
liquid. These heat exchanger are also used when the operating temperature or pressure is high or we have
fouling fluids in our system. Following are the classification of such kind of heat exchanger:
A double pipe heat exchanger contains of one pipe concentrically inside another large diameter pipe. The
major use of double pipe heat exchangers is for sensible heat and cooling of process fluids, where the small
heat transfer areas are required.
Shell and tube heat exchangers are typically made of round tubes mounted in cylindrical shell with a tube
axis parallel to that of shell. One fluid flows inside the tubes, while other fluid flows across and along the
tube. This type of exchanger were majorly used in petroleum, petrochemical and fertilizer industry. For an
effective heat transfer, a large heat transfer area should be used, leading to the use of many tubes.
The BPA is flammable, corrosive in nature. Shell and tube heat exchanger is excellent for handling
flammable and corrosive fluids. So, we select shell and tube exchangers because:
It is less expensive and providing maximum heat transfer surface per given surface and tube size.
It provides multi-tube flow arrangement.
Shell and tube exchanger is able to handle high operating temperature.
Floating end allow for differential thermal expansion between shell and the tubes. Moreover, tube bundles
can be easily repaired and replaced.
This configuration gives a large surface area in a small volume.
When designing the shell and tube exchanger, we will careful about some guidelines:
The corrosive fluid should be placed at tube side.
The fluid most likely to be cause fouling is placed at tube side.
The tubes should made from a corrosion resistant material. This is much less expensive than having a shell
made from this material, if corrosion occurs, only the tubes needs to be replaced.
Usually, the hotter fluid is placed at tube side, and the cooler fluid usually placed at shell surrounding the
tubes.
4.1.4 Design of a Heat Exchanger
The flow rates for both the fluids were calculated by applying material balance.
As, we have Bisphenol A – water system and we are going to cool the BPA using water . As ,BPA will
place at TUBE side and water will placed at SHELL side.
Heat duty
Q = m Cp ∆T Q = m Cp ∆T
As in our system, we are using water services for bisphenol A . Choose 1inch at outer diameter and .01338m
as inner diameter. Selecting 8BWG and assuming square pitch having pitch (Pt=1*1/4 inch).
(T1−t2)−(T2−t1)
LMTD = T1−t2 ,
ln( )
T2−t1
∆Tm = Ft × ∆Tln
Ft - Correction factor.
𝑇 −𝑇 (𝑡 −𝑡 )
R = (𝑡1−𝑡2) S = (𝑇2 −𝑡1 )
2 1 1 1
R = 0.4092 S = 0.722
20.449
Ft =
20.925
Ft = 0.95
As, Ft is greater than 0.75 which means our heat exchanger is thermally suitable and we should use 1-2 pass
heat exchanger.
∆Tm = Ft × ∆Tln
∆Tm = 72.96°C
Q = U × A × ∆Tm
68380
A = (500)∗72.96
A = 1.87 m2
Number of tubes and tube size
Choose 0.015875 m as tube outer diameter and 0.0133858m as tube inside diameter. Assuming that length
of tubes is 10ft (3.048 m).
Area of 1 tube = π × l × do
1.87
Number of tubes= Nt = 0.1519
Nt 1
Db= do (K1)n1
16
Db= 15.875 (0.175)1/2.285 = (115 mm)
Figure 6. Bundle Diameter Clearance [1].
Use a fixed and U-tube head type in above figure, bundle diametrical clearance is 15mm. Shell diameter,
Ds = 115+ 15 = 130mm ..
The value of n1 and K1 is obtained from table below:
1000/3600 kg
Fluid mass velocity = 5.62∗10^−4 = 494.24 m2 s
494.24
Fluid linear velocity = = 0.5 m/s
971.8
ℎ𝑖 𝑑𝑖 𝜇
= .023 × 𝑅𝑒^.8 × 𝑃𝑟 0.33 × ( )0.14
𝑘 𝜇𝑤
ρ×u×di
Re = μ
971.8×0.5×0.013385
Re = = 18635
.355×10−3
𝜇
Neglect (𝜇𝑤)0.14
So, hi = 3740 W/m2°C
hio=hi*ID/OD=3153 W/m2°C
Pt /do=1.25
Ds=220mm Bs =Ds/5=44mm
(Pt−do)Ds lb
Cross flow area = = 1.94*10^-3 m2
Pt
867.13/3600
Mass velocity = Gs = = 124.16 kg/m2sec
1.94∗10^−3
1.1
Equivalent diameter = de = do ( Pt 2 − 0.907 do2 )
de = 0.0114 m
G×de 124.16×0.0114465
Re = = = 568.4
μ 0.25 ×10−3
Jh = 1.95*10^-2
k μ
hs= de × jh × Re × Pr 0.33 × (μw)0.14
𝜇
Neglect (𝜇𝑤)0.14
hs = 260 W/m2°C
𝑈 500
Across water film = ℎ𝑠 × ∆𝑇 = 260.11 × 88.4 = 170°C
0.25
(.355)0.14 = 0.9520
hs = 247.67 W/m2°C
Overall coefficient:
Taking the fouling coefficient from table below. For organic as heat transfer
Uo=525.56 W/m2°C
As, we assumed overall heat transfer co-efficient, U = 500 W/m2 °C as our first estimate. Our calculated
value (i.e. 525.26 W/m2 °C) is greater than assumed value.
Area required
68380
A = (525)∗72.96
A = 1.79 m2
jf = 5.5 × 10−3
Density=971.8kg/m3
𝜇 0.14
( ) =1
𝜇𝑤
𝐿 𝜇 𝜌𝑢𝑡 2
∆Pt = 𝑁𝑝 [8 × 𝑗𝑓 × × (𝜇𝑤)−𝑚 + 2.5] ×
𝑑𝑖 2
3.048 𝜇 (971.8)∗0.52
∆Pt = 4 [8 × (5.5 × 10−3 ) × × (𝜇𝑤)−𝑚 + 2.5] ×
.0133858 2
∆Pt = 171.55pa=0.17kpa
jf = 8×10−2
Ds L ρus2 μ
∆Ps = 8 × jf × de × lb × × (μw)−0.14
2
∆Ps = 5423.97pa=5.42kpa
Both shell and tube pressure drops were lies in a limit of 10 psi. So that is why we have satisfactory operation.
According to kern, this is quite adequate design as we were assuming that there is no leakages and bypasses.
Design of A Mixing Tank
STEP#1
Volume of Tank
V = Td * Q
V= 331.5m3
Assume two tanks of 165.75 m3 each are installed in parallel, we will calculate
the design parameters of only one tank which will be identical to the otherone.
STEP#2
Ideally,
L/D=1
Now,
As,
D=L
So,
D= 5.95 m
STEP # 3
Dia Of Impeller
STEP # 4
Agitator Selection
As, we have
rps =2
STEP # 5
P =K* ρ * N3 * D5
Reynolds Number
Re = (D2 *N *ρ)/ µ
Where,
D = diameter of impeller N
= rotations per second ρ=
density of wastewater
µ= viscosity of waste water
Putting values in above relation, we have
P= 39.6 Kw
ii
Kinetic study of adductive crystallization of bisphenol-A By A. Alamdari ∗, S. Shariat Nasab, A. Jahanmiri
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
iii
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
iv
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
v
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
vi
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
vii
Kinetic study of adductive crystallization of bisphenol-A By A. Alamdari , S. Shariat Nasab, A. Jahanmiri
∗
viii
Characterization of Crystal Size Distribution by Angelo Chianese
ix
Bisphenol A Adduct under the influence of impurities byEhsan Eurfokan and almadari
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Principle of mass transfer Binny K Dutta
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US 6960697 patent
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Basic design for Crystalization
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Chemical Engineering Plant design 6th edition Richardson Coulson