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13

CO Distillation in Structured Packing

Physical 3D models were established for corrugated packing used in the enrich-

ment of the isotope

13

C. Computational fluid dynamics (CFD) simulation results

indicated that common corrugated packing was not well wetted when used for

isotope distillation. It is concluded that liquid misdistribution in the packed

tower results from the structure of the packing rather than from the height of the

packing beds. The existence of entrainment was also demonstrated by CFD simu-

lation. It is proved that mass transfer equations based on the Nusselt theory are

not suitable for distillation calculation in such a corrugated packing system. By

comparison, the recently developed structured packing model with a corrugation

geometry based on the right-angled triangle, known as Zigzag-pak, describes

vapor-liquid distribution properties well and has significant advantages over

common corrugated packing due to its better liquid distribution character.

Keywords: Corrugated packing, Cryogenic distillation, Isotope

13

C, Transfer intensification,

Zigzag-pak

Received: July 15, 2011; revised: November 01, 2011; accepted: November 02, 2011

DOI: 10.1002/ceat.201100273

1 Introduction

The stable isotope

13

C is widely used as a tracer element in the

fields of medicine, pharmacology, and organic chemistry. In

particular, the rapid rise of the

13

C breath test in clinical diag-

nosis has gradually replaced the radioactive

14

C breath test over

recent years. There are several methods for producing

13

C,

including thermal diffusion, chemical exchange, gas diffusion,

laser, and cryogenic distillation, with the latter being the only

industrial technique. CH

4

and CO can be used in cryogenic

distillation [13], and their separation factors are 1.0035

1.0054 and 1.0071.01, respectively. In order to obtain 99 %

13

C from the natural abundance of 1.11 % needs about 3000

theoretical stages which necessitates industrial distillation col-

umns with lengths of more than 100 m [4, 5]. On the other

hand, such manufacturing devices are difficult to scale up

because of a significant shortcoming, i.e., the random packing

utilized in the columns.

Structured packing has been applied to the separation of

isotopes because of its good gas-liquid distribution properties

compared with random packing [6]. However, unfortunately

there is little understanding of the phenomenon of two-phase

distillation in the narrow channels of the packing. In order to

improve the phase exchange on the surface of structured pack-

ing, the common method is to increase the specific surface

area of packing. This is based on the Nusselt theory which

assumes that the liquid flows as a thin film over the whole sur-

face of the packing. Thus, one can conclude that the vapor-liq-

uid interfaces are in positive ratio to the surfaces of the pack-

ing. However, no one has confirmed by measurement that the

falling film retains a stable thickness for fully developed flow in

the channels of corrugated packing when used for

13

CO distil-

lation.

A corrugated gauze packing, called PACK-

13

C, with a

specific surface area of 1135 m

2

m

3

was fabricated and used in

a

13

C-enriching pilot-scale plant through carbon monoxide

(CO) cryogenic distillation [7]. The packing bed was 18 m

high, and the column diameter was 45 mm. The packing per-

formed well regarding its mass transfer properties with more

than 20 theoretical stages per meter. The cryogenic installation

has a capacity of producing about 2.1 g of 15 %

13

C per day. It

is difficult to continuously increase the specific surface area of

packing because of the difficult manufacture and operation.

Therefore, it is of critical importance to study the gas-liquid

distribution in the corrugated gauze packing in order to

improve the mass transfer efficiency. However, little attention

has been paid to the two-phase flow distribution on the surface

of structured packing. Because of the construction of narrow

channels for corrugated gauze packing, it is extremely difficult

to carry out experimental measurements on the behavior of

this type of countercurrent flow. Previous research has simply

modeled the corrugated packing as large plate, measured the

www.cet-journal.com 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim Chem. Eng. Technol. 2012, 35, No. 2, 334340

Hu-Lin Li

1,2

Yong-Lin Ju

1

Liang-Jun Li

2

Da-Gang Xu

2

1

Shanghai Jiao Tong University,

Institute of Refrigeration and

Cryogenics, Shanghai,

China.

2

Shanghai Research Institute of

Chemical Industry, Shanghai,

China.

University, Institute of Refrigeration and Cryogenics, 800 Dongchuan

Road, Shanghai 200240, China.

334 H.-L. Li et al.

liquid flow, and simulated its flow by computational fluid

dynamics (CFD) methods [8]. One report solved the empirical

equations to obtain the parameters of mass transfer efficiency

[9, 10]. Others have calculated the pressure drop through

structured packing by CFD simulations [11]. These studies

proposed the application of CFD simulations in packed

towers. In this paper, CFD simulations were carried out to

study the two-phase flow in the narrow channels of corrugated

packing. Based on the CFD simulation, a new type of corru-

gated packing with better liquid distribution properties,

known as Zigzag-pak, has been proposed and manufactured.

Parameters of the common corrugated packing and zigzag

packing are listed in Tab. 1.

2 Mathematical Models

The volume-of-fluid- (VOF) model can develop two or more

immiscible fluids by solving a single set of momentum equa-

tions and tracking the volume fraction of each of the fluids

throughout the domain [12]. In the current simulation, the

VOF model is used to calculate the properties of the CO vapor

and CO liquid that flow as countercurrents in the corrugated

packing channels. The two CO phases are treated as incom-

pressible fluids in the packing channels and the RNG-based

k-e turbulence model is used for the numerical simulation.

The renormalization group (RNG) model has an additional

term in its e equation that significantly improves the accuracy

for rapidly strained flows. The effect of swirl on turbulence is

included in the RNG model, enhancing the accuracy for swir-

ling flows. The RNG theory provides an analytically derived

differential formula for effective viscosity that accounts for the

effects of low Reynolds numbers. These features make the

RNG k-e model more accurate and reliable for two-phase

vapor-liquid flows in the narrow channels of the structured

packing than the standard k-e model.

2.1 Volume Fraction Equation

The tracking of the interfaces between the phases is accom-

plished by the solution of a continuity equation for the volume

fraction of the two phases. For the q

th

phase, the equation is:

1

q

q

t

a

q

q

q

_ _

a

q

q

q

~v

q

_ _

_ _

n

p1

_ m

pq

_ m

qp

(1)

where q is the volume-averaged density. The q

th

fluid volume

fraction in the cell is denoted as a

q

, _ m

qp

is the mass transfer

from phase q to phase p, and _ m

qp

is the mass transfer from

phase p to phase q.

2.2 Momentum Equation

t

q~v q~v~v p l ~v ~v

T

_ _ _

q~g

~

F (2)

where p is the static pressure, ~v is the component of the flow

velocity parallel to the gravitational vector, l is the viscosity, g

is the gravitational acceleration, and

~

F is the external body

force.

2.3 Energy Equation

t

qE ~vqE p k

eff

T (3)

in which k

eff

is the effective thermal conductivity. The VOF

model treats the energy, E, and the temperature, T, as mass-

averaged variables.

2.4 Closure Equations

The RNG k-e turbulence model is derived from the instanta-

neous Navier-Stokes equations, using a mathematical tech-

nique called the renormalization group (RNG) method. The

analytical derivation results in a model with constants different

from those in the standard k-e model, and additional terms

and functions in the transport equations for k and e.

t

qk

x

i

qku

i

x

j

a

k

l

eff

k

x

j

_ _

G

k

G

b

qe (4)

t

qe

x

i

qeu

i

x

j

al

eff

e

x

j

_ _

C

1e

e

k

G

k

C

3e

G

b

C

2e

q

e

2

k

Re

(5)

where R

e

is given by

R

e

C

l

qg

3

1 g=g

0

e

2

1 bg

3

e

2

k

(6)

In these equations, G

k

represents the genera-

tion of turbulence kinetic energy due to the

mean velocity gradients, and G

b

is the genera-

tion of turbulence kinetic energy due to buoy-

ancy. The quantities a

k

and a

e

are the inverse

effective Prandtl numbers for k and e, respec-

tively. g = Sk/e, g

0

= 4.38, and b = 0.012.

Chem. Eng. Technol. 2012, 35, No. 2, 334340 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com

Table 1. Comparison of two types of corrugated gauze packing.

Packing types Peak height

[mm]

Wave length

[mm]

Hydraulic

diameter

[mm]

Porosity Area

[m

2

m

3

]

Common corrugated

packing

2.5 4 2.8 0.77 1100

Zigzag-pak 2.5 2.5 1.3 0.62 1900

Transfer intensification 335

3 Geometry and Boundary Conditions

Structured packing has a complicated geometric construction,

and, therefore, needs a lot of time and physical memory to

solve the above dynamic equations even for the calculation of

one packing element. In the current paper, the simulation

model is based on one triangular channel from a piece of the

packing element. The boundary conditions are as follows: the

inlet velocity of the gas is 0.743 ms

1

, the outlet pressure of the

gas is 60 kPa, the inlet velocity of the liquid is 0.0013 ms

1

, and

the outlet boundary of the liquid is the outflow. The tempera-

ture is 80 K, and the fluids are the two phases of CO.

Fig. 1 is a schematic of the common corrugation geometry

of the packing used in the

13

C distillation installation. The cor-

rugation height is 2.5 mm, the corrugation width is 4 mm, and

the side length is 3.2 mm.

Fig. 2 presents schematically the new corrugation geometry

Zigzag-pak, where the corrugation height is 2.5 mm and the

corrugation width is 2.5 mm. The main difference in geometry

between the Zigzag-pak and common packing is that the for-

mer has a right-angled triangle corrugation whereas the latter

has an isosceles triangle corrugation.

The schematic diagrams of the current CFD models

for the common packing and the new Zigzag-pak are

illustrated in Figs. 3 and 4, respectively. They both have

the same corrugation inclination angle of 45 and the

same length of flow channel with 50 mm. As shown in

Figs. 3 and 4, there is one inlet velocity for gas, one

inlet velocity for liquid, one outlet pressure for gas,

one outflow for liquid, two walls, and one symmetry

boundary for each 3D model.

4 Experiments

A commonly used corrugated gauze packing,

PACK-

13

C, with a specific surface area of 1135 m

2

m

3

was installed in the CO cryogenic distillation column

[13]. The PACK-

13

C was fabricated by compressing a

double-layer silk screen, made of stainless steel, into

the corrugated shape. Pieces of the screens were then

assembled with an inclination angle of 45, corruga-

tion height of 2.5 mm, porosity of 0.77, and silk diameter of

0.085 mm. The packing bed was 18 m high, and the diameter

of the packing was 45 mm. When the F-factor varied from 0.18

to 0.90 ms

1

(kg m

3

)

1/2

, the numbers of theoretical stages per

meter ranged between 20 and 30. In that case, the pressure

drop was less than 25 Pa for one theoretical plate, the dynamic

liquid holdup was between 11 % and 21 %, and the pilot-scale

plant produced 2.1 g of 15 %

13

C per day. The experimental

measurements demonstrated that the PACK-

13

C exhibited a

higher mass transfer efficiency than traditional random pack-

ing when used for

13

C distillation.

As demonstrated in the flow sheet of Fig. 5, the purified CO

gas flowed into the cryogenic distillation column at the feeding

point, the extracted gas was removed at the top of the column

by a vacuum pump, and the concentrated

13

C product was taken

out at the bottom of the column. The

13

CO was enriched by

numerous liquid-vapor exchanges on the surface of the packing.

The column was well insulated using multilayer insulation, and

the total heat leakage of the column was less than 30 W. Raw

materials were high-purity CO gas and commercial liquid nitro-

gen. The CO vapor and liquid nitrogen exchanged heat in the

condenser located on the top of the column, and the vaporized

nitrogen gas was drawn out by a pump. The installation real-

ized automatic operation and ran smoothly for over six

months.

5 Simulation Results and Discussion

The CFD simulations were carried out using the Fluent 6.3

software platform. In this solver, a first-order upwind scheme

and pressure-velocity coupling algorithms were applied for the

discretization of differential equations. The two-phase fluids of

liquid CO and vapor CO flow as countercurrents in the com-

mon corrugated packing installed in the cryogenic column.

The operation conditions were the same as those in the experi-

ments. The distribution of liquid phase in the common corru-

gated gauze packing is displayed in Fig. 6.

www.cet-journal.com 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim Chem. Eng. Technol. 2012, 35, No. 2, 334340

Figure 1. Geometry of the common corrugated packing.

Figure 2. Geometry of the newly developed packing Zigzag-pak.

Figure 3. 3D model for the common corrugated packing.

336 H.-L. Li et al.

Liquid CO streams down on one side of the chan-

nel even though it spreads out as a thin film on the

inlet surface. Most of the packing surfaces are not

moistened. This does not agree with the common

opinion which assumes that liquids cover uniformly

all of the packing surfaces. Therefore, the CFD simu-

lation proves that large areas are not wetted and the

liquid is not well distributed in a distillation column

filled with common corrugated packing. It is clear

that this structural limitation can lead to liquid mis-

distribution. Previously, liquid misdistribution has

often been considered as the result of too high pack-

ing beds. It is concluded that it is not appropriate to

simplify the packing element as a large plane, as pre-

vious reports have done, although these have vali-

dated the flow behavior on the plates by experimental

measurements. The reason is that liquids are more

sensitive to the structure of the flowing channels than

gases. In short, fluid flow in the channels of the cor-

Chem. Eng. Technol. 2012, 35, No. 2, 334340 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com

Figure 4. 3D model for the new Zigzag-pak.

vacuum

pump

vacuum

pump

purification

column

waste

gas

rotameter

high vacuum

pump

product

coolant

CO cylinder

cryogenic-

destillation

column

liquid

nitrogen

tank

nitrogen

gas

structured

packing

P

P

P

P

P

H

H

Figure 5. Flow sheet of the

13

C cryogenic installation.

Transfer intensification 337

rugated packing cannot be studied by simplifying it as a large

plane plate.

In comparison, the CFD simulation for CO countercurrent

flow in the Zigzag-pak packing is given in Fig. 7. The wavy liq-

uid film flows downward and spreads to both sides of the

downside wall. The surfaces are evenly covered by liquid,

which is more consistent with the assumption of the mass

transfer calculations. As a result, the moistened surfaces of this

packing are much larger than those of common packing, and,

therefore, the mass transfer is intensified.

The pressure drop along the y-direction on the symmetry

surface of the Zigzag-pak is plotted in Fig. 8. The result is simi-

lar to the experimental result using common corrugated pack-

ing.

Unlike common corrugated packing, the liquid distribution,

plotted in Fig. 9, indicates that much of the liquid film is

located in the outlet of the right-angled triangle channel of the

Zigzag-pak. Because the liquid distribution is optimized in the

Zigzag-pak, there are larger vapor-liquid interfaces for mass

exchange for the same gross packing volume than for common

packing. Thus, the mass transfer is certainly intensified in the

Zigzag-pak channels.

Fig. 10 displays the particle path lines of the vapor and liq-

uid in the Zigzag-pak for

13

CO cryogenic distillation.

From the above CFD simulations, the details of the vapor-

liquid flow in the structured packing are clearly indicated, i.e.,

liquid misdistribution in the packed towers probably results

from the structural limitation of the packing, and the liquid

misdistribution is independent of the height of the packing

beds. Although the common corrugated packing used for

13

C

separation in tests proved to be superior to traditional random

packing, it has a serious geometrical limitation. The newly

developed Zigzag-pak with a corrugation geometry consisting

of a right-angled triangle has a better liquid distribution char-

acter and could be applied in distillation towers to replace the

common corrugated packing to provide higher mass transfer

efficiency.

6 Conclusions

A simplified 3D physical model representing the corrugated

packing element is established and solved by computer. These

CFD simulations illustrate that the common corrugated pack-

ing is not well wetted in precision distillation because of its

structural limitation. It has been proved that the mass transfer

equations, based on the Nusselt theory, are not suitable for dis-

tillation calculation in such a corrugated packing system. Liq-

uid misdistribution in the packed towers results from the

structure of the packing rather than from the height of the

packing beds. The new type of corrugated packing, the Zigzag-

pak, with right-angled triangle corrugation has a better liquid

distribution character and larger vapor-liquid interfaces than

those of the common corrugated packing. Considering its

prominent advantages in vapor-liquid intensification and high

www.cet-journal.com 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim Chem. Eng. Technol. 2012, 35, No. 2, 334340

Figure 6. Distribution of liquid CO in the common corrugated

packing.

Figure 7. Distribution of liquid CO in the Zigzag-pak.

Figure 8. Pressure drop along the y-direction on the symmetry

surface of Zigzag-pak.

338 H.-L. Li et al.

efficiency in mass transfer, the Zigzag-pak could replace com-

mon corrugated packing in chemical engineering.

Acknowledgment

This research has been financially supported by the Shanghai

Science and Technology Talent Project in China (No.

10QB1401700). The experiments were carried out in the labo-

ratory of the Shanghai Engineering Research Center for Stable

Isotopes.

The authors have declared no conflict of interest.

Symbols used

_ m [kg s

1

] mass flow rate

p [Pa] static pressure

E [J] total energy

T [K] temperature

k

eff

[Wm

1

K

1

] effective thermal conductivity

~

F [N] force vector

g [ms

2

] gravitational acceleration

G

k

[] generation of turbulence kinetic energy

due to the mean velocity gradients

G

b

[] generation of turbulence kinetic energy

due to buoyancy

S [J K

1

] total entropy

t [s] time

k [J kg

1

] kinetic energy per unit mass

u [ms

1

] velocity magnitude

~v [ms

1

] overall velocity vector

C

1e

[] constant, 1.42

C

2e

[] constant, 1.68

C

3e

[] constant, 0.0845

Greek symbols

q [kg m

3

] density

g [] effectiveness factor

l [Pa s] dynamic viscous

a

p

[] p

th

fluid volume fraction

a

q

[] q

th

fluid volume fraction

a

k

[] inverse effective Prandtl numbers for k

a [] inverse effective Prandtl numbers for e

l

eff

[Pa s] effective viscosity

e [m

2

s

3

] turbulent dissipation rate

Subscripts

q q

th

phase

p p

th

phase

Chem. Eng. Technol. 2012, 35, No. 2, 334340 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com

Figure 9. Contours of liquid volume

fraction on the surface of the liquid out-

let for Zigzag-pak.

Figure 10. Particle path lines for the vapor and liquid in Zigzag-

pak.

Transfer intensification 339

References

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[2] A. Rdoi, M. Gligan, S. Dronca et al., Conf. on Isotopic and

Molecular Processes, Cluj-Napoca, Romania, September 1999.

[3] T. Monguchi, Chem. Equip. 2001, 7, 7.

[4] K. Takashi, K. Hitoshi, H. Shigeru et al., Nippon Sanso Com-

mun. 2004, 23, 20.

[5] H. L. Li, Y. L. Ju, L. J. Li et al., J. Labelled Compd. Radio-

pharm. 2010, 53, 342.

[6] H. L. Li, L. J. Li, S. N. Li et al., Low Temp. Spec. Gas. 2008, 6,

9.

[7] H. L. Li, Y. L. Ju, L. J. Li et al., At. Energy Sci. Technol. 2009,

Suppl., 54.

[8] A. Hoffmann, I. Ausner, J. U. Repke et al., Comput. Chem.

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[9] Z

1999, 38, 683.

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[11] M. H. Fard, M. Zivdar, R. Rahimi et al., Chem. Eng. Technol.

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340 H.-L. Li et al.

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