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1

Department of Automatic Control

26-28 Gh. Baritiu Str., 400027 Cluj-Napoca, Romania

http://aut.utcluj.ro

e-mail: clement.festila@aut.utcluj.ro

Abstract- The industrial distillation plants- like those for crude

oil- and the cryogenic distillation column for (13C) isotope enrichment have in common the probability to appear an undesirable

phenomenon: the flooding, when the plant efficiency decreases

drastically. After a general description of the isotope separation

problem, the paper describes the column mode of operation and

gives the mathematical equations, which explain the column flooding process. The authors deal with the online prediction methods

and propose a simple, low-cost method based on the supervision of

the process variables: differential column pressure (top-bottom)

and liquid level in boiler (variables, first and second derivatives).

Using a test-version of the column, where the flooding can be observed directly, the method proposed by the authors proves its

utility.

Keywords: (13C) cryogenic distillation, flooding, pattern recognition, prediction

I. INTRODUCTION

Isotopes are species of the same element with different number of neutrons in the nucleus. For instance, the chemical element carbon consists of the basic species (12C) and the

heavier stable isotope (13C) with a ratio of natural concentration of (98.89% / 1.11%) [1,2]. If some chemical compounds of

carbon with higher concentration in (13C) isotope in detriment

of (12C) can be obtained, the detection of those chemical compounds brings valuable quantitative and qualitative information

in various domains: chemical engineering, biology, medicine,

etc.

A great variety of technologies able to create compounds

with higher abundance in the isotope of interest are known today. In the case of (13C) one of these is the cryogenic distillation.

The separation process analysis is based on the hydrodynamic process- specific for each separation technology- and

the separation process itself, relatively independent of the

technology used.

II. PRINCIPLE OF THE SEPARATION METHOD

Unfortunately, the physical and chemical properties of the

compounds of (12C) and (13C) are very close, being difficult to

separate. Even though, very small differences in properties

must be used to raise the concentration of (13C) to separate

the isotope of interest. For instance, at very low temperatures

( 190D C ) the carbon monoxide based on (12C) has a higher

vapor pressure (p) than the monoxide based on (13C). It is possible to find and to maintain a small range of temperature in

which the gaseous phase (related to (12C)) coexists with the

liquid phase (based on (13C)). It is necessary to distillate the

compounds (12CO versus 13CO) in a distillation column like in

the typical industrial distillation equipment [3]: the gaseous

phase must be evacuated and the liquid phase which contains

a greater abundance of 13CO - is kept as end-product. The basic

factor is the separation coefficient [1], given by the ratio

of the vapor pressures:

=

pD13 CO

pD12 CO

>1

(1)

with = 1.011 , pD13 CO the vapor pressure of 13CO and pD12 CO the

vapor pressure of 12CO.

This particular isotope separation technology is called

cryogenic distillation.

III. BASIC EQUIPMENT DESCRIPTION

The equipment is called cryogenic distillation column,

figure 1, and is divided for simplicity- in three parts [3]: the

boiler (B) on the bottom side, the condenser (C) at the top side

and the packed distillation column (tower). The external

flows are: the feed flow (F), the waste flow (W) and the product flow (P).

In the column, an upward vapor (gas) stream, generated by

the evaporation in the boiler is brought into contact with a

downward flowing stream of liquid produced by condensation

in the condenser zone. The boiler is heated with an electrical

resistor and the condenser is cooled with liquid nitrogen. During this permanent contact, the concentration of (13CO) increases in the liquid phase in the column basis. The packing material

inside the column increases the contact surface between the

liquid and the gaseous phases. In order to flow up from the

boiler to the condenser, the vapor stream needs some effective

area through the elements of the packing material. This area is

greater by dry packing material and smaller by wet material.

The gaseous upstream needs a differential pressure along the

column. Every liquid droplet is submissive to the force of gravity and, in the opposite direction, to the pressure force of the

gas. In normal mode of operation, the gravity is stronger and

the liquid phase flows as droplets to the boiler.

the packing material increases and the column is no longer effective in washing away the undesired component from the

gas [7,8]. The gas pressure and liquid quantity impedes proper

gas transit and the liquid droplets are suspended on the packing material. This phenomenon - the flooding reduces drastically the column efficiency and can compromise the whole

process of isotope separation.

The general particularity of the isotope separation process is

the huge ratio between the feed flow-rate and the final product

flow-rate (F/P >>). An imposed column efficiency: shorter

separation time/higher isotope enrichment, leads to a higher

charge of the column: greater flow rates (F,W), more thermal

energy in boiler, etc. But the column capacity is limited and by

surpassing the certain values of operational variables, many

undesired states may occur, the most frequent being the flooding. Thus, the column operates under stress.

IV. HYDRODYNAMIC PROCESS, BASIC ASSUMPTIONS, FLOODING

In normal mode of operation, the gaseous phase is assumed

to flow upward inside the numerous small channels having

the same characteristic dimensions. The liquid phase flows

down the fictious walls of the channels and reduces the

available cross-sectional area for the gas flow, thus causing a

pressure drop (a differential pressure p ). The pressure variations may be caused by other disturbances: feed material

quality/ composition, temperature distribution, flow-rates

changes, etc.

An operation of the isotope separation column with as high

as possible charge (flow rates, heating and cooling energy) is

desired, but under these circumstances, the possibility to onset

the flooding increases, with disastrous consequences. A flooding predictor, in the ideal case, will keep the column point of

operation close to the flooding (higher efficiency), but in a safe

area. If some input/ internal variables change and the flooding

can appear, the predictor alarms the operator - in open loop - or

even gives a control signal- in closed loop- to avoid future

flooding. So, the flooding predictor can be viewed as an advanced process control strategy that utilizes a pattern recog-

to increase the stability and energy efficiency of the column

operation.

More methods to predict flooding onset are known today,

methods that can be divided in offline and online ones. For

instance, for packed distillation columns (also valid for isotope

separation columns) several offline empirical/ analytical flooding models exist [4]:

a. generalized pressure drop correlation (GPDC);

b. suspended-droplet models;

c. double-film models;

d. flooding velocity ( us ) prediction;

e. pressure drop correlation, etc.

For all these methods, numerous experimental data are necessary to determine the values of the main parameters. Based

on these models, the calculated and the measured values of

the variables are compared, the results being used to refine the

models. Of course, the heat losses and the apparatus indications

may be the source for differences.

The online methods use both the static and the dynamic

models of the column [5]. One supposes the availability of the

measurements of differential pressure ( pk ), liquid level in

the boiler ( h B ), feed flow rate ( Fk ), etc and it is possible to

calculate (online, using the process computer) their derivatives:

p , h B , etc) in order to ensure the predictive capability

( p ,

of the model. The structure of the static column model able to

give the predicted differential pressure ( p ) with the prediction horizon of (k) is given in figure 2. The efficiency of the

prediction may be evaluated using the correlation factor (R),

well known in stochastic system analysis.

Dynamic models use the current inputs and their derivatives

and the past values of the main variables (like p ) to predict

the output ( p ) at (t+k).

Figure 3 gives the dynamic model principle of implementation for ( p ), using one-step and m-step time delay.

TABLE 1

DIFFERENTIAL PRESSURE FUNCTION OF ELECTRICAL POWER IN THE BOILER

In order to improve the prediction, the actual output (differential pressure p ) is compared with the predicted value p(t + k ) . The measured value p(t ) , filtered by

H 1 (s ) (low pass filter) is compared with the estimated value y (t ) . The prediction error, (t ) , smoothed by H 2 ( s) , is

added to the predicted value p(t + k ) in order to obtain the

COLUMN: EXAMPLES

If (t ) is the flow rate of the gaseous phase for carbon monoxide and ( Rh ) is the hydrodynamic resistance, in a simplified version one supposes that:

k el Pel

(2)

1 / Rh = a b Pel

(3)

and

Pel (p.u.)

p (p.u.)

k

b3 4

b2 3

b 2

= el Pel + k el

Pel =

Pel + k el

Pel + k el

a

a4

a3

a2

= a1 Pel + a 2 Pel2 + a3 Pel3 + a 4 Pel4

(4)

flow rate, the differential pressure ( p ) for different values of

the electrical power ( Pel ) is given in table 1.

87

109

140

210

230

340

If the derivative ( p / Pel ) would be available, results:

D p ( Pel ) = 1.48 + 0.46 Pel 1.09 10 2 Pel2 +

+ 6.92 10 5 Pel3

(5)

The technical solution of the column permits to detect the

flooding and this was observed by Pel 85( p.u.) .

The measured pressure evolution and the values obtained by

interpolation are given in figure 5. The evolution of the derivative ( p / Pel ) is given in figure 6. It is not difficult to observe three different slopes:

(p / Pel )1 = 0.0834

(p / Pel ) 2 = 0.0582 (normal mode)

350

measured values

interpolation polynomial

300

Differential pressure (p.u.)

1

k el Pel

b

b 2 2 b 3 3

k el +

Pel +

Pel +

Pel Pel =

a a2

a b Pel

a3

a4

74

By polynomial interpolation, with fourth order approximation, the following values of the coefficients are obtained:

( k el , a, b ) are proper coefficients. Using the long division method, the pressure drop is given by: the equation:

p =

44

250

200

150

100

40

50

60

70

80

Electrical power (p.u.)

90

100

110

the slope of the derivative has a much greater value:

0.331 >> 0.0582

VI. SIMPLIFIED VERSION OF THE FLOODING PREDICTOR BASED

ON ESTIMATOR

column, the flooding phenomenon may be predicted by the

supervision of the slope ( dp / dPel ) using the differential

(p) k and (Pel ) k .

The simplified algorithm is given by the following set of equations:

pk pk 1

(6)

1.

Pel , k Pel ,k 1

(7)

2.

3.

4.

= p k p k 1

D

Pel , k Pel ,k 1

>

D

< (D)

lim

(8)

(9)

figure 7.

VII. CONCLUSIONS

The disastrous consequences of the flooding phenomenon in

distillation column justify the theoretical and practical effort of

the specialists in order to predict/avoid this process. The general solution, at least according to actual references, is the predictive control theory and methods. In the particular case of the

cryogenic distillation for (13C) separation, where the information for the temperature distribution in the column is not available, accurate and prompt information about the differential

column pressure using commercially available transducers and

about the liquid level in the boiler, using a patented modern

transducer [6], the evolution of the first and second derivative

of these variables can predict and avoid the column flooding.

The solution is modern, effective and low-cost.

ACKNOWLEDGMENT

The authors acknowledge the support of the Romanian National Education and Research Ministery under PN2 Grant

81023/14.09.2007.

REFERENCES

[1]

[2]

[3]

[4]

[5]

[6]

Figure 6. Evolution of the differential pressure derivative

[7]

[8]

Gh. Vasaru, Stable Isotopes, (in Romanian), Editura Tehnica, Bucuresti 1968

D. Axente, M. Abrudean, A. Baldea, Isotope Separation 15N, 18O, 10B,

13

C through Isotope Exchange, (in Romanian), Casa Cartii de Stiinta,

1994

S. Skogestad, Dynamics and Control of Distillation Columns- a Tutorial

Introduction, Trans IChemE Symposium on Distillation and Absorption,

part A, pp. 539-562, Maastricht, September 1997

X-C. Fang, Z-M Cheng, L. Huang, Z-X. Liu, B-P. Han, R-H. Zeng and

W-K. Yuan, Prediction of Flooding Velocity in a Trickle Bed, International Journal of Multiphase Flow, Vol. 31, Issue 5, pp.666-673, May

2005

S. Parthasarathy, H. Gowan and P. Indhar, Prediction of Flooding in an

Absorbtion Column using Neural Networks, in Proceedings of the IEEE

International Conference on Control Applications, pp. 1056-1061, Hawai, 1999

M. Gligan, E. Dulf, M.L. Unguresan and Cl. Festila, Preliminaries Regarding General Modeling of Cryogenic Distillation with Application to

(13C) Isotope Separation, in Proceedings of the IEEE International Conference on Automation, Quality and Testing, Robotics, tome I, pp. 155159, Cluj-Napoca, May 2006

M. G. Mphahlele, R.B. Eldridge, Distillation Column Flooding Predictor, in Proceedings of The AIChE Spring National Meeting, Advances in

Distillation Modeling and Processes, topical 8, Orlando, 2006

S.C da Silva, E. Nicolaievsky, L.C Santos and C.L.C. Costa, Evaluation

of Flooding in Batch Distillation Columns, in Proceedings of the 2nd

Mercusor Congress on Chemical Engineering, ENPROMER, vol. 1, Rio

de Janeiro, 2005

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