Distillation and Heating Time Calculation1111

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Batches often are concentrated by applying heat from steam in a jacket (or similar means).

Common references such as Kern’s

Equally unhelpful, batch distillation literature primarily focuses on predicting component splits via vapor/liquid equilibrium and th

BATCH CONCENTRATION
Figure 1. Equation assumes liquid continues to contact the straight sides of the vessel.

DERIVING THE EQUATION


For simplification, let’s assume the liquid is in a jacketed tank and remains on the straight side of the vessel as it is concentrate

First, let’s consider the geometry of the batch as it remains on the tank straight side:

The wetted area is:

AS = πDh (1)
The volume relationship is:
VS = πD2h/4 (2)
Dividing Eq. 1 by Eq. 2 provides the area-to-volume relationship:
AS/VS = 4/D (3)
So, the total wetted area is:
AT = AH + 4(VT-VH)/D (4)
Differentiating Eq. 4 with respect to time gives:
dAT/dt = (4/D)dVT/dt (5)

Next, let’s write an alternative expression for dVT/dt using the heat transfer rate and fluid properties:

dVT/dt = -Q/(ρΔH) (6)

Substituting the standard expression for heat transfer yields:


dVT/dt = -UATΔT/ρΔH (7)

Using Eq. 5 to eliminate volume in the relationship leads to:


(D/4)dAT/dt = -UATΔT/ρΔH (8)

Solving for dAT/dt gives:


dAT/dt = -4UATΔT/ρDΔH (9)

At this point, it is convenient to define a characteristic time constant:


Θ = ρDΔH/4UΔT (10)

Substituting Eq. 10 into Eq. 9 gives:


dAT/dt = -AT/Θ (11)

Rearrangement yields:
dAT/AT = -dt/Θ (12)

We then can solve Eq.12 per standard procedure:


dln(AT ) = -1/Θdt (13)

Integrating to the indefinite solution gives:


ln(AT) = -t/Θ (14)
Then, substituting the integration limits (At at time t, A0 at time 0), we obtain:
ln(At/A0) = <-t/Θ (15)

Rewriting Eq. 15 provides the following simple equation:


At/A0 = e–t/Θ (16)
where Θ is given by Eq. 10.

PROCESS EXAMPLE
We want to concentrate a batch from 735 gal to 617 gal in a 5-ft-diameter tank. The bottom head holds 74 gal and provides 23

First, we must convert volumes to cubic feet:


V0 = 735/7.481 = 98.25 ft3 2.242
Vt = 617/7.481 = 82.48 ft3 1.652
VH = 74/7.481 = 9.89 ft3 0.59 m3

Then, we calculate wetted areas per Eq. 4:

A0 = 23 + 4(98.25 - 9.89)/5 = 93.7 ft2 Volume ofVH = 0.098966 D3 =


0.00
At = 23 + 4(82.48 - 9.89)/5 = 81.1 ft2
Area of BAH =0.927D =0.00
2

From Eq. 10, we determine characteristic time:


Θ = (62.3 × 5 × 1,036)/(4 × 50 × 165) = 9.78 hr

Using a rearrangement of Eq. 15 we get:

t = -Θ ln(At/A0) = - 9.78 ln(81.1/93.7) = -9.78 ln(0.8655) = 1.4 hr


So, the time needed to concentrate the batch from 735 gallons to 617 gallons is 1.4 hr.

MICHAEL J. GENTILCORE is Hazelwood, Mo.-based chemical process engineering manager for Mallinckrodt, a business unit

NOMENCLATURE
A Area, ft2
D Tank diameter, ft
h Liquid height above head, ft
ΔH Heat of vaporization, Btu/lb
Q Heat transfer rate, Btu/hr
ΔT Temperature difference between jacket and process, °F
t Time, hr
U Overall heat transfer coefficient, Btu/(hr∙ft2∙°F)
V Volume, ft3

ρ Liquid density, lb/ft3


Θ Time constant (per Eq. 10), hr

Subscripts
0 Time zero
H Bottom head
S Straight side of vessel
T Total
t Time t

REFERENCES
1. Kern, D. Q., “Process Heat Transfer,” p. 624, McGraw-Hill, New York (1950) [still available in McGraw-Hill Classic Textbook R
2. Green, D. W. and Perry, R. H., “Perry’s Chemical Engineers’ Handbook,” 6th Ed., p. 10-38, McGraw Hill, New York (1997).
3. Gentilcore, M. J., “Estimate Heating and Cooling Times for Batch Reactors,” p. 41, Chem. Eng. Progress (March 2000).
on references such as Kern’s “Process Heat Transfer” [1] and “Perry’s Chemical Engineers’ Handbook” [2] cover transient heating and coolin

apor/liquid equilibrium and the Rayleigh Equation. No publication appears to offer a quick way to predict the time needed to distill or evapora

e vessel as it is concentrated (Figure 1). For purposes of integration, let’s also assume the heat of vaporization (ΔH), liquid density (ρ), ove
olds 74 gal and provides 23 ft2 of wetted area, in addition to the jacket. The solvent has a heat of vaporization of 1,036 Btu/lb and a density

m3

m2

Mallinckrodt, a business unit of Covidien that will become a standalone company in 2013. E-mail him at [email protected]
Graw-Hill Classic Textbook Reissue Series].
aw Hill, New York (1997).
Progress (March 2000).
over transient heating and cooling, as does an earlier paper of mine [3]. However, their unsteady-state analyses treat wetted area as a con

time needed to distill or evaporate a batch to a desired concentration. This article introduces just such an equation.

tion (ΔH), liquid density (ρ), overall heat transfer coefficient (U) and the temperature differential between the steam or other heat-transfer m
on of 1,036 Btu/lb and a density of 62.3 lb/ft3. We can assume the overall heat transfer coefficient is 50 Btu/(hr∙ft2∙°F). What is the time to e

[email protected]
lyses treat wetted area as a constant, which clearly isn’t the case when a batch is boiled down.

e steam or other heat-transfer medium in the jacket and the liquid in the tank (ΔT) remain constant.
u/(hr∙ft2∙°F). What is the time to evaporate the batch if the ΔT across the jacket is maintained at 165°F?
Distillation Time
Distill out the IPA Calculations
under vacuum(NLT 650 mmhg) @50-55°C
(semi solid residue is observed )

Initial Vol. of Reaction Mass V0 = 5.419


Final Vol. of Reaction Mass Vt = 0.741

Bottom dish to be 10% Torispherical Dish

Volume of Bottom Dish VH = 0.098966 D3 = 1.29

Area of Bottom Head AH =0.989987D2 = 5.48

Initial wetted area is: A0 = AH + 4(V0-VH)/D 12.50


Area Based On F
Final wetted area is: At = AH + 4(Vt-VH)/D 4.48 Volume present
reactor

Area of Bottom Head

Density of Solvent ρ= 785


Latent heat of Vaporization of Solvent λ = 172.39
Overall Heat Transfer Coefficient U= 300
Vessel diameter D= 2.35

ΔT for Hot water ΔT= 11.43

Characteristic time constant: Θ = ρDλ/4UΔT = 23.21

Time Required for Distillation t = -Θ ln(At/A0) = 23.80


m3
m3

Initial
Temp. of Final Process Temprature Temprature
Process
Hot Water Temperature approach approach
Temperature

∆T1 = T1-t2
T1 t1 t2 ∆T2 = T1-t1
m3 °C °C °C °C °C

m2 65 52 55 13 10

m2
Area Based On Final
2242
2 Volume present in the
m 1652
reactor

Kg/m3
KCal/kg
Kcal/hr m2°C
m

°C

hrs

hrs
Logarthmic
temperature
difference

∆TLMTD =
(∆T1-∆T2)
Ln (∆T1/∆T2)
°C

11.43
««« back
Diketone
Reactor-9004 10 KL
Heating Time and Distillation Time Calculations

Heating the Reaction Mass from 30 to 55°C for Distillation

Non Isothermal Heating


Reactor Contents
Mass M 4760
Initial temp t1 30
Final temp t2 55
Sp.Heat Cm 0.67
Area A 20.9
HTC U 300 Assumed 4°C
Temperature dr
hot water
Heating Fluid(HOT Water)
Inlet temp T1 60
Sp.Heat Cw 0.99
Flow rate W 20132.70

Time required for heating

ln T1 - t1
T1 - t2

K = e(UA/WC)

K 1.37
Time reqd =

Distillation Time
Distill out the IPA Calculations
under vacuum(NLT 650 mmhg) @50-55°C
(semi solid residue is observed )
Area Based On F
Volume present
reactor
Initial Vol. of Reaction Mass V0 = 5.419
Final Vol. of Reaction Mass Vt = 0.741
reactor

Bottom dish to be 10% Torispherical Dish

Volume of Bottom Dish VH = 0.098966 D3 = 1.29

Area of Bottom Head AH =0.927D2 = 5.13

Initial wetted area is: A0 = AH + 4(V0-VH)/D 12.15

Final wetted area is: At = AH + 4(Vt-VH)/D 4.19

Area of Bottom Head

Density of Solvent ρ= 785


Latent heat of Vaporization of Solvent λ = 172.39
Overall Heat Transfer Coefficient U= 300
Vessel diameter D= 2.35

ΔT for Hot water ΔT= 11.43

Characteristic time constant: Θ = ρDλ/4UΔT = 23.21

Time Required for Distillation t = -Θ ln(At/A0) = 24.71


Kg
°C
°C
Kcal/Kg °C
m2
KCal/hr m2 4°C
Assumed °C
Temperature drop of
hot water

°C
Kcal/Kg °C
Kg/hr

= WCw x K-1 xt
MCm K

1.062 hrs

Area Based On Final


Volume present in the
reactor
m3
m3
reactor

Initial
Temp. of Final Process Temprature Temprature
Process
Hot Water Temperature approach approach
Temperature

∆T1 = T1-t2
T1 t1 t2 ∆T2 = T1-t1
m3 °C °C °C °C °C

m2 65 52 55 13 10

m2
2242
m2 1652

Kg/m3
KCal/kg
Kcal/hr m2°C
m

°C

hrs

hrs
Logarthmic
temperature
difference

∆TLMTD =
(∆T1-∆T2)
Ln (∆T1/∆T2)
°C

11.43
««« back
HBS

Heat the reaction mass to 87±5°C.

Non Isothermal Heating


Reactor Contents
Mass M 9257 Kg
Initial temp t1 20 °C
Final temp t2 87 °C
Sp.Heat Cm 0.6698 Kcal/Kg °C
Area A 20.9 m2
HTC U 300 KCal/hr m2 °C

Heating Fluid
Inlet temp T1 92 °C
Sp.Heat Cw 0.99 Kcal/Kg °C
Flow rate W 20000 Kg/hr

Time required for heating

ln T1 - t1 = WCw x K-1 xt
T1 - t2 MCm K

K = e(UA/WC)

K 1.372544981
Time reqd = 3.08 hrs
Proposal of Using Steam instead of Hot Water

Isothermal Heating
Reactor Contents
Mass M 9257 Kg
Initial temp t1 20 °C
Final temp t2 87 °C
Sp.Heat Cm 0.6698 Kcal/Kg °C
Area A 20.9 m2
HTC U 400 KCal/hr m2 °C

Heating Fluid
Inlet temp T1 133.34 °C

Time required for heating

ln T1 - t1 = U A time
T1 - t2 MC

Time reqd = 0.66 hrs


39.8 min

Steam at @3Kg/cm2
(2 Kg/cm2 gauge Pressure + 1 Kg/cm2 atmospheric pressure)

B.Point Temperature @ 3 Kg/Cm2 133.34 °C


Batches often are concentrated by applying heat from steam in a jacket (or similar means). Common references suc
their unsteady-state analyses treat wetted area as a constant, which clearly isn’t the case when a batch is boiled do

Equally unhelpful, batch distillation literature primarily focuses on predicting component splits via vapor/liquid equilib
introduces just such an equation.

BATCH CONCENTRATION
Figure 1. Equation assumes liquid continues to contact the straight sides of the vessel.

DERIVING THE EQUATION


For simplification, let’s assume the liquid is in a jacketed tank and remains on the straight side of the vessel as it is c

First, let’s consider the geometry of the batch as it remains on the tank straight side:

The wetted area is:

AS = πDh (1)
The volume relationship is:
VS = πD2h/4   (2)
Dividing Eq. 1 by Eq. 2 provides the area-to-volume relationship:
AS/VS = 4/D  (3)
So, the total wetted area is:
AT = AH + 4(VT-VH)/D (4)
Differentiating Eq. 4 with respect to time gives:
dAT/dt = (4/D)dVT/dt  (5)

Next, let’s write an alternative expression for dVT/dt using the heat transfer rate and fluid properties:

dVT/dt = -Q/(ρΔH)  (6)

Substituting the standard expression for heat transfer yields:


dVT/dt = -UATΔT/ρΔH (7)

Using Eq. 5 to eliminate volume in the relationship leads to:


(D/4)dAT/dt = -UATΔT/ρΔH  (8)

Solving for dAT/dt gives:


dAT/dt = -4UATΔT/ρDΔH (9)

At this point, it is convenient to define a characteristic time constant:


 Θ = ρDΔH/4UΔT   (10)

Substituting Eq. 10 into Eq. 9 gives:


dAT/dt = -AT/Θ (11)
Rearrangement yields:
dAT/AT = -dt/Θ   (12)

We then can solve Eq.12 per standard procedure:


dln(AT ) = -1/Θdt (13)

Integrating to the indefinite solution gives:


ln(AT) = -t/Θ (14)

Then, substituting the integration limits (At at time t, A0 at time 0), we obtain:
ln(At/A0) = <-t/Θ (15)

Rewriting Eq. 15 provides the following simple equation:


At/A0 = e–t/Θ (16)
where Θ is given by Eq. 10.

PROCESS EXAMPLE

We want to concentrate a batch from 735 gal to 617 gal in a 5-ft-diameter tank. The bottom head holds 74 gal and p
transfer coefficient is 50 Btu/(hr∙ft2∙°F). What is the time to evaporate the batch if the ΔT across the jacket is maintai

First, we must convert volumes to cubic feet:


V0 = 735/7.481 = 98.25 ft3
Vt = 617/7.481 = 82.48 ft3
VH = 74/7.481 = 9.89 ft3

Then, we calculate wetted areas per Eq. 4:


A0 = 23 + 4(98.25 - 9.89)/5 = 93.7 ft2
At = 23 + 4(82.48 - 9.89)/5 = 81.1 ft2
AT = AH + 4(VT-VH)/D
From Eq. 10, we determine characteristic time:
Θ = (62.3 × 5 × 1,036)/(4 × 50 × 165) = 9.78 hr

Using a rearrangement of Eq. 15 we get:

t = -Θ ln(At/A0) = - 9.78 ln(81.1/93.7) = -9.78 ln(0.8655) = 1.4 hr
So, the time needed to concentrate the batch from 735 gallons to 617 gallons is 1.4 hr.

MICHAEL J. GENTILCORE is Hazelwood, Mo.-based chemical process engineering manager for Mallinckrodt, a business unit

NOMENCLATURE
A Area, ft2
D Tank diameter, ft
h Liquid height above head, ft
ΔH Heat of vaporization, Btu/lb
Q Heat transfer rate, Btu/hr
ΔT  Temperature difference between jacket and process, °F
t Time, hr
U Overall heat transfer coefficient, Btu/(hr∙ft2∙°F)
V Volume, ft3

ρ Liquid density, lb/ft3


Θ  Time constant (per Eq. 10), hr

Subscripts
0 Time zero
H Bottom head
S Straight side of vessel
T  Total
t   Time t

REFERENCES
1. Kern, D. Q., “Process Heat Transfer,” p. 624, McGraw-Hill, New York (1950) [still available in McGraw-Hill Classic
2. Green, D. W. and Perry, R. H., “Perry’s Chemical Engineers’ Handbook,” 6th Ed., p. 10-38, McGraw Hill, New Yor
3. Gentilcore, M. J., “Estimate Heating and Cooling Times for Batch Reactors,” p. 41, Chem. Eng. Progress (March 2
emperature differential between the steam or other heat-transfer medium in the jacket and the liquid in the tank (ΔT) remain con
uid in the tank (ΔT) remain constant.

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