E. Simeonov, J.

Nedialcova Journal of the University of Chemical Technology and Metallurgy, 41, 4, 2006, 445-448

PROCESS CONTROL AND ESTIMATION OF MULTISTAGE EXTRACTION USING CHARACTERISTIC FUNCTION APPROACH
E. Simeonov, J. Nedialcova

University of Chemical Technology and Metallurgy 8 Kl. Ohridski, 1756 Sofia, Bulgaria E-mail: evgeni@uctm.edu

Received 05 September 2006 Accepted 12 November 2006

ABSTRACT Kinetic experiments have been carried out, under three-stage led process of extraction according to the scheme crossed current, for the system tobacco leaves (Nicotiana tabacum L.) water. The solid phase is triple extracted and a fresh solvent is used for each stage. The experiments are obtained in a batch extractor with a propeller. The characteristic function for the experimental system is obtained from the kinetic curves. By using this function the basic design size (length) of solid liquid extractor is calculated. The new working speed (II and III stages) of solid stage transition in the extractor is also obtained, which is done by screws rpm and constant design sizes calculated from the kinetic curves for the Ist stage of the extraction. The obtained revolutions correspond to the necessary equilibrium time of extraction, which is the time of reaching the reference extraction degree of the extracted component. Keywords: solidliquid extraction, kinetics, characteristic function, multistage extraction.

INTRODUCTION The efficiency of extraction installations is usually estimated by technological criteria the degree of extraction. According to the need of quality refining of raw materials and reaching high extraction degree, the solid phase refining is usually multistage and the number of stages is defined for each particular case. It is well known that each experimental kinetic curve holds in hidden way all the factors that have an impact on the process of non-stationary diffusion extraction [1-4]. Kinetics by the characteristic function gives the opportunity in the common case for polydisperse anisotropic solid phase, the characteristic in the structure of solid particles and the value of the external diffusion resistance to be integrally found [3,6].

The use of the characteristic function gives possibility not only to calculate but also to control the process [7] when the raw material is changed, the technological parameters of the multistage extraction. EXPERIMENTAL Kinetic experiments have been carried out, under three-stage led process of extraction according to the scheme crossed current for the tobacco leaves water system. The solid phase has been extracted three times and fresh solvent has been used for each stage. The experimental data have been obtained in a batch vessel extractor with a propeller under the following conditions: hydromodule =0,02 m3/kg, temperature t=200C and stirring revolutions n=7 s-1, for which have been

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Journal of the University of Chemical Technology and Metallurgy, 41, 4, 2006

proved that the external diffusion resistance has been eliminated. The concentration trend of the extracted substances in the liquid phase versus time was recorded during the experiments. Weighting was used for measuring the concentrations with up to 10-3 g accuracy, after drying the samples at 700C. The initial concentrations are defined by experiments, too. The initial concentrations of the solid phase is C0=607.97 kg/m3 and the saturation concentration is C*=801.04 kg/m3. RESULTS AND DISCUSSION The experimentally obtained results for the investigated solid-liquid system are shown in Fig. 1 and can be described with acceptable accuracy with equation (1). From the presented results can be seen that a peak in the concentration curves for the second and third stage of extraction is observed. The reason for this is the more rapid obtaining of the equilibrium concentrations with the increasing the number of the extraction stages. When designing the extraction apparatuses the kinetic curve section, where the velocity is the biggest i.e. to ensure certain stay of the material at a given extraction stage, is of any interest. The bigger velocity of the process is due to the quickly increasing internal porosity of the solid phase. C1=A-Bexp(-H) (1)

maximum of concentration for stage II and stage III shown as Fig. 1.

Fig.1. Experimental kinetics curves in a stirred batch apparatus.

The standard function [8] for each stage is defined in equations (5), (6), and (7).

* ( ) = 1,027 1,0244. 2,5051.10 ( ) = 1,1642 1,0522. 9,654.10

*

(5) (6) (7)

( ) = 1,545 1,0461. 9, 7698.10

*

The conditions that equations (5), (6), and (7) are derived are: C0 = 607,97, kg / m3 , C1 = 22,20g / m3 and = 0,0370 . It is well known that the representations of the experimental data using the standard function give the ability to predict the kinetics when there is a change in the phase ratio () and an internal diffusion regime. The conditions and the sequence for defining the characteristics function are discussed in detail in [5, 6]. Equation (2) gives kinetics information for the investigated material derived in batch vessel extractor with a propeller and =0,02 m3/kg. Using the standard function (5) the data is recalculated for working hydromodule in continuous screw extractor - =2,604 m3/kg. The predicted kinetic curves for all the three stages are shown in Fig. 2.

where A, B, H are numerically defined on the basis of the experimental results. The following equations are obtained from (1) for each of the stages (I, II and III)

C1 = 22,20 22,10. 2, 60.10 C1 = 8,47 7,56. 9, 79.10 C1 = 2,47 1,29. 9,81.10

3

(2) (3) (4)

Equations (3) and (4) describe the experimental results only up to the time necessary for reaching the

( ) =
1

d ( )

(8)

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E. Simeonov, J. Nedialcova

Fig. 2. Calculated kinetics curves in a continuous apparatus.

Fig. 4. Relationship between process kinetic and design. Characteristics in a screw extractor for system I.

Fig. 3. Sequence for obtaining function ().

where:

( ) = 1 m0 De

dF

De, m2/s coefficient of diffusion ( ) - Characteristic function relative solid mass reduction The sequence system shown in Fig. 3 is used to obtain equation (8). The following system of equations (9) is used to calculate periodical and continuous processes:

Fig. 5. Main design characteristics of the screw conveyer.

d ( ) = C C1 ( ) d

(9)

(1 ) 1 = C1 ( ) C m
It is also used to define the residence time of substances in the extractor under the following conditions =2,604 m3/kg, Cm=0,172 kg/m3, C1n=0.

solving of ( ) and ( ) / time in the extractor/ is derived the function ( ) for counter-flow in continuous extractor Fig. 4. The screw length (Fig. 4) of continuous screw extractor is calculated on the following conditions: solid phase productivity G=11,57.10-3kg/s, external porosity of the solid phase in the space between screw grinds sc=0,91m3/m3, material density c=928 kg/m3. At any time there is corresponding value of h: h=w (11)

d 1 1 0 C C m [ ( )]

(10)

Where w is the speed of the solid phase in the extractor w=

The equation is numerically solved by linear point on Simpsons method. The necessary extraction time and the corresponding reference degree of leaching are also found. After the elimination of at co-

G c f sc (1 sc )

(12)

as shown in Fig. 4 the necessary length of the screw for the Ist stage of extraction is h=2,555 m.

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Journal of the University of Chemical Technology and Metallurgy, 41, 4, 2006

Table 1. Main parameters in the screw extractor operation.

eq
Stage I-st II-nd III-rd

d sc

w.10 3

s m
0,112 0,112 0,112

N .10 2 s 1
2,535 5,703 7,604

z
pcs.
23 23 23

s
900 400 300

m
0,249 0,249 0,249

m/ s
2,839 6,388 8,517

m
2,555 2,555 2,555

It shows the abilities of the characteristic function for defining the new necessary speed of solid phase for passing through the extractor (new screw revolu tions N= eq s ) and reaching the reference degree of leaching. In Table 1 are shown the derived values for more important technological parameters for all three stages of extraction. The calculations are made on main construction sizes base obtained from the Ist extraction stage. Table 1. Main parameters in the screw extractor operation. CONCLUSIONS Three-stage extraction kinetics is investigated in the counter-flow scheme for tobacco leaves water system. Kinetics curves for each stage are obtained in a batch stirred vessel extractor. The standard and characteristic function for the investigated system are calculated. The ability of the characteristic function for process controlling is demonstrated for three stage extraction of the solid phase. When there are constant screw dimensions, the necessary screw revolution is defined. They guarantee that the real time of staying corresponds to the reference degree of leaching. Acknowledgement The authors would like to thank the Science & Research Programme of the University of Chemical

Technology and Metallurgy for the financial support (Project 10266). REFERENCES 1. E. Simeonov, A.Minchev, Kinetics of multistage extraction from vegetable raw materials, J. Univ. Chem. Technol. Met. (Sofia), !&, 1, 2003, 91-98. 2. . Simeonov.,I.Tsibranska, A.Minchev, Solid-liquid extraction from plants- experimental kinetics and modeling, Chemical Engineering Journal, %!, 1999, 255-259. 3. E. Simeonov, I.Seikova,Evaluation of the Variable Internal Porosity During Solid-Liquid Extraction, Bulg. Chem. Commun., vol.!#, 2003, 2. 4. I. Seikova.E.Simeonov, E.Ivanova, Protein Leaching from Tomato Seed- Experimental Kinetics and Prediction of Effective Diffusivity, Journal of Food Engineering, $, 2004, 165-171. 5. E. Simeonov, I.Seikova, I.Penchev, A.Minchev, ScaleUp of the Solid-Liquid Extraction Using Characteristic Function Technique, Ind. Eng. Chem. Res., "!, 2004, 4903-4907. 6. P. Romankov, G.; V. Frolov, Mass transfer in chemical technology, Chimia, St. Petersburg, USSR, 1990, 126-134, (in Russian). 7. E. Simeonov, A.Minchev, Calculation and Control of Solid-Liquid Extraction with Characteristic Function, Russ. Journal of Applied Chemistry, % , 4, 2003, 544-546. 8. G. Axelrood, Mass transfer in solid-liquid system; Lvov, USSR, 1970, 115-131

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