WCE2010 pp709-714
WCE2010 pp709-714
WCE2010 pp709-714
Generic motor of variable velocity with direct transmission from 0 rpm to 1,500 rpm, 60
1 Hertz, 127 VCA , agitation arrow of 14 inches (length) and diameter of ¼ inch, in stainless
steel 316
Agitator/impeller of four rectangular ring with separation of 90° among each cross.
1
Crosses’ longitude of 2 inches x 1inch of length for largeness in stainless steel 316.
2 Thermocouple J type. From 0 °C to 760 °C, wire-rope: 3 m.
1 Thermo-well in copper of 14 inches (length) and diameter of ½ inch.
Thermal isolation for high temperature with glass fiber of thickness ½ inch and recovered
1
with paper aluminum foil.
Programmable recirculating bath (Julabo F-34), temperature range from -34 °C to 200 °C,
1
pump flow of 15 Lpm, bath volume from 14 L to 20 L and 120 VCA/60 Hz.
Digital tachometer ACT-3. Monarch Instrument. Measurement range from 5 rpm to 999
1 990 rpm with accuracy of 0.0015% +/ - 1 rpm, 4-20 mA or 0-5. V, sensitivity of 0.5 ms and
optic sensor of infrared ray with range from 1 rpm to 250 000 rpm.
1.354
1.352 Fig. 5 shows the experimental density-temperature
1.350
1.348
relationship where the critical points of MSZW are located
1.346 by considering the minimum temperature for each
1.344
1.342
temperature range presented in the Table 2. The density
1.340 corresponding to every saturation temperature was located
1.338
25 30 35 40 45 50 55 60 65 70
considering the Fig. 2 that presents the density averages of
Temperature (蚓 ) the experimental runs. From Fig. 5, we can observe that the
Fig. 2 Average density in function of cooling down of 1 zones width (metastable and labile) increases of non-linear
°C. form as the saturation temperature (cooling) decrease in a
range from 70 to 40 °C. Meade and Chen [21] reported that
The saturation line (equilibrium) was obtained from (1) as the width for each zone for a cane sugar solution is constant
a function of density: and linear along the same cooling temperature range.
However, our results showed that this is not the case,
sat 1.33 8.89 10 5 T 6.91 10 6 T 2 becoming a contribution for understanding of the saturation
(2) line, metastable zone and labile zone.
where sat is the saturation density in g/cm3 for each specific A non-linear second order regression was applied to the
equilibrium temperature. The density interval for a experimental data presented in the Fig. 5. The modeling
temperature range from 70 to 40 °C is from 1.3594073 to equations describe the intermediate limit of the metastable
1.3392435 g/cm3, respectively. zone and the limit of starting of the labile or unstable zone.
B. CSD and Micrographs Analysis Specifically, the intermediate line with R2= 0.998 is given by:
Fig. 3 shows the experimental data of the CSD in % int ermediate 1.32 5.39 10 4 T 8.32 10 8 T 2
volume with a log-normal distribution for each saturated (3)
solution (40, 50, 60 and 70 °C), being this the most where intermediate is the density in the intermediate limit of the
representative with regard to the average of three metastable zone in g/cm3. The density interval of the model
experimental runs for every saturation temperature. The by a temperature range from 70 to 40 °C is from 1.36148 to
analysis of this figure is based on the quantification and 1.34502 g/cm3, respectively. The labile line can be describing
observation of patterns on the crystal population for both according to the fitted equation with R2= 0.998:
cooling temperature and density range. In accordance with
100 100
90 90
80 80
70 70
% Volume
60
% Volume
60
50 50
40 40
30 30
20 20
10 10
40 50
0 38 0
36 48
50 50
100 34 ) 100 46 )
150
32 (蚓 150 44 ( 蚓
Siz 30 re Siz re
e(
m
200 28 atu e(
m
200
42 ratu
250 26 er ) 250 e
)
mp mp
300 24 Te 300 40 Te
a b
100 100
90 90
80 80
70 70
% Volume
60 60
% Volume
50 50
40 40
30 30
20 20
10 10
60 70
0 0
50 58 68
100 100 66
56 ) 64
150 蚓 200 )
e(
200 54 62 (蚓
300
Siz 250 ur 60 re
e(
m 300 52 rat Siz
e (蚓 400 58 tu
e ra
) 350 mp ) 500 56
mp
e
400 50 Te 600 54 Te
c d
Fig. 3 CSD of saturated solutions at: a) 40 °C, b) 50 °C, c) 60 °C and d) 70 °C.
Fig. 4. Micrographic sequence of growth crystals in saturated solution to 40°C. a) first metastable zone (40-37 °C), b) second
metastable zone (36-33 °C) and c) labile zone (32 °C or smaller).
Unstable line
3
1.3550
zo
ne crystallizer. Chem. Biochem Eng. Q 16 (3). 125-129.
1.3525 ble
sta
[6] Mersmann, A. Crystallization Technology Handbook; Marcel Dekker:
1.3500 eta New York. 1995.
nd M ne
2 zo
1.3475 ble [7] Velazquez-Camilo, O., Alvarez-Ramirez, J. J. and Bolaños-Reynoso,
sta
eta E. (2009). Comparative Analysis of the Crystallizer Dynamics Type
1.3450 st M
1.3425
1 Unsaturated zone Continuous Stirred Tank: Isothermic and Cooling Case. Rev. Mex. Ing.
Quim. (RMIQ). 8 (1). 127-133.
1.3400
[8] Salcedo-Estrada L. I., Quintana-Hernandez, P. A. and
1.3375 Bolaños-Reynoso E. (2002). Mathematical Modeling in Batch
30 35 40 45 50 55 60 65 70
Crystallization. Chem. Eng. Assoc. Chem. Eng. Uruguay 3(21). 3-11.
Temperature (蚓 )
[9] Christofides P. D., Shi D., El-Farra N. H., Li M. and Mhaskar P. (2006).
Fig. 5 Metastable and labile zone limits (MSZW) at the Predictive control of particle size distribution in particulate processes.
Chemical Engineering Science. 61. 266-280.
density – temperature diagram.
[10] Rawlings J. B. and Miller S.M. (1994). Model identification and
control strategies for batch cooling crystallizers. AIChe Journal. 40 (8).
labile 1.32 8.32 104 T 3.7 106 T 2 (4) 1312-1327.
[11] Bolaños-Reynoso Eusebio, Xaca-Xaca Omar, Alvarez-Ramirez Jose,
and Lopez-Zamora Leticia. (2008). Effect Analysis from Dynamic
Where labile is the density of starting limit of the labile zone Regulation of Vacuum Pressure in an Adiabatic Batch Crystallizer
Using Data and Image Acquisition. Ind. Eng. Chem. Res. 47 (23),
in g/cm3. The density interval of the model by a temperature 9426-9436.
range from 70 to 40 °C is from 1.36269 to 1.34992 g/cm3, [12] Fujiwara Mitsuko, Nagy Zoltan K., Chew Jie W. and Braatz Richard D.
respectively. Eqs. (3) and (4) shows clearly that the (2005). First-principles and direct design approaches for the control of
pharmaceutical crystallization. Journal of Process Control. 15.
concentration limits are non-linear functions of temperature. 493-504.
[13] Zhou George X., Fujiwara Mitsuko, Woo Xing Yi, Rusli Effendi, Tung
IV. CONCLUSION Hsien-Hsin, Starbuck Cindy, Davidson Omar, Ge Zhihong, and Braatz
Richard D. (2006). Direct Design of Pharmaceutical Antisolvent
The identification of the critical points of MSZW for Crystallization through Concentration Control. Crystal Growth &
commercial sugar cane was made in this work. A novel Design. 6 (4). 892-898.
experimental method, based on cooling down sugar cane [14] Hanks, J. Counting Particles of Cells using IMAQ Vision; Software is
the Instruments, Application Note 107; National Instruments, Inc:
solutions and micrographs evaluation was used, yielding a Austin, TX, 1997.
close description of the concentration limits for the saturation [15] Wang, X. Z.; Calderon-De-Anda, J.; Roberts, K. J. (2007). Real-Time
line, the first and second metastable zone, and labile zone in Measurement of the Growth Rates of Individual Crystal Facets using
Imaging and Image Analysis. A Feasibility Study on Needle-Shaped
density terms. In contrast to commercial practice, we found Crystals of L-Glutamic Acid. Trans. IChemE, Part A, 85, 921–927.
that the width of the zones increases in a non-linear form as [16] Calderon-De-Anda, J.; Wang, X. Z.; Roberts, K. J. (2005). Multi-scale
the cooling saturation temperature decreases from 70 to 40 Segmentation Image Analysis for the In-Process Monitoring of
Particles Shape with Batch Crystallizers. Chem. Eng. Sci. 60,
°C. The MSZW obtained experimentally should be useful for 1053–1065.
the design and operation of industrial crystallization [17] Cordova-Pestaña, N. M.; Bolaños-Reynoso, E.; Quintana-Hernandez,
equipment oriented to obtain specific products. P. A.; Briseño-Montiel, V. M. Developing of CSD Analysis Software
from Electronic Microscopy Measurement; XXV AMIDIQ’s
Memories: Mexico. 2004.
ACKNOWLEDGMENT [18] Rawle, A. Basic Principles of Particle Size Analysis; Technical Paper
We thank Amira Antonio Acatzihua (CONACYT’s MS Ref. WR141AT; Malvern Instruments: U.K., 1999.
[19] Quintana-Hernandez, P. A.; Moncada-Abaunza, D. A.;
scholarship) for her collaborations in this paper. Bolaños-Reynoso, E.; Salcedo-Estrada, L. I. (2005). Evaluation of
Sugar Crystal Growth and Determination of Surface Area Shape
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[20] MasterSizer S Long Beb’s User Manual; Malvern Instruments. Ltd.:
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7a edition, McGraw-Hill. 2001. [21] Meade, G. P. and Chen, J. C. Cane Sugar Handbook: A Manual for
[2] Quintana-Hernandez, P., Bolaños-Reynoso, E., Miranda-Castro, B. and Cane Sugar Manufacturers and their Chemists. Wiley Publisher. 1977.
Salcedo-Estrada, L. (2004). Mathematical Modeling and Kinetic
Parameter Estimation in Batch Crystallization. AIChE Journal. 50 (7).
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