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Characterization of micromixing in a Continuous Oscillatory Baffled Reactor

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HAL Id: hal-02373265

https://hal.archives-ouvertes.fr/hal-02373265

Submitted on 22 Nov 2019

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Characterization of micromixing in a Continuous Oscillatory Baffled Reactor

M. Avila, M Poux, C Xuereb, D. Fletcher, Joelle Aubin

To cite this version:

M. Avila, M Poux, C Xuereb, D. Fletcher, Joelle Aubin. Characterization of micromixing in a Contin- uous Oscillatory Baffled Reactor. 16th European Conference on Mixing, Sep 2018, Toulouse, France.

�hal-02373265�

(2)

Variation of the segregation index with the oscillatory Reynolds number

cs Nitech© glass reactor Operational conditions and solution concentrations

Characterization of Micromixing in a Continuous Oscillatory Baffled Reactor

M. AVILA 1 , M. POUX 1 , C. XUEREB 1 , D.F. FLETCHER 2 , J. AUBIN 1

1 Laboratoire de Génie Chimique, Université de Toulouse, CNRS, INPT, UPS, Toulouse, France

2 School of Chemical and Biomolecular Engineering, The University of Sydney, NSW 2006, Australia

Micromixing performance

• Micromixing performance is determined by the Villermaux–Dushman reaction system [4], based on a set of competing parallel reactions:

𝐻

2

𝐵𝑂

3

+ 𝐻

+

↔ 𝐻

3

𝐵𝑂

3

Eq. (1) Quasi-instantaneous.

5𝐼

+ 𝐼𝑂

3

+ 6𝐻

+

↔ 3𝐼

2

+ 3𝐻

2

𝑂 Eq. (2) Very fast

𝐼

2

+ 𝐼

↔ 𝐼

3

Eq. (3) Quasi-instantaneous equilibrium

Parameter Value

Reactor diameter (𝐷) 15 mm Orifice diameter (𝑑

0

) 7.5 mm Tee pipe diameter (𝑑) 0.4 mm Baffle spacing (𝑙

𝑏

) 16.9 mm Oscillation frequency (𝑓) 0.5 – 1.5 Hz Oscillation amplitude (𝑥𝑜) 2.8 – 12.68 mm

Flow rate ratio (𝑅) 3.63 7.26 Main flow rate (𝑄

𝑛𝑒𝑡

) 4.68 kg/h

Influence of acid concentration and oscillatory conditions Influence of flow rate ratio

Continuous oscillatory baffled reactors (COBRs) offer interesting advantages over traditional mixing processes in stirred tanks, such as effective mixing, good mass and heat transfer in laminar and transitional flow [1], as well as plug flow with long residence times. These characteristics have been shown to improve liquid-liquid reactions [2] and crystallization processes [3].

Whilst numerous works on the characterization of COBRs have focused on the study of flow patterns, velocity profiles and RTD [4], or the conversion rate of some reactions [2, 5], there is little quantified knowledge on the macro- and micromixing performance of these reactor types. Indeed, COBRs are most often used in applications where the kinetics are slow. However, micromixing performance in the COBR is of interest for applications with initial fast reactions or precipitations that also require long residence time (for consecutive reactions or crystal/precipitate growth). Such applications are still challenging because the COBR typically does not provide fast micromixing conditions, thereby leading to local segregation and a decreases in selectivity and/or product properties.

The objective of this work is to study the effect of the oscillatory conditions in the Nitech® COBR in the laminar flow regime (𝑅𝑒

𝑜

< 2000) on micromixing performance using the iodide-iodate or Villermaux- Dushman test reactions [6].

Reactant Concentration [M]

H

3

BO

3

0.1818

NaOH 0.0909

KIO

3

0.00233

KI 0.0116

H

2

SO

4

0.03 0.015 0.0075

• The greater the yield of I

2

, the poorer the micromixing quality.

• Determination of product concentration through spectrophotometry.

• Mixing efficiency measured by the segregation index, 𝑋

𝑆

:

𝑋

𝑠

= 𝑌

𝑌

𝑇S

= 𝐻

+

𝑚𝑜𝑙𝑒𝑠 𝑐𝑜𝑛𝑠u𝑚𝑒𝑑 𝑏𝑦 𝑒𝑞. (2)

𝑆𝑒𝑙𝑒𝑐𝑡𝑖𝑣𝑖𝑡𝑦 𝑜𝑓 𝑖𝑜𝑑𝑖𝑑𝑒 𝑤ℎ𝑒𝑛 𝑡ℎ𝑒𝑟𝑒 𝑖𝑠 𝑡𝑜𝑡𝑎𝑙 𝑠𝑒𝑔𝑟𝑒𝑔𝑎𝑡𝑖𝑜𝑛

• Same reactant molar flow rates in both cases [7-8] .

• Same trend of 𝑋

𝑠

with 𝑅𝑒

𝑜

for both flow rate ratios R

• 𝑋

𝑠

decreases with an increase in acid flow rate.

• Influence of injection flow: Increase of instabilities in the injection zone from 𝑅𝑒

inj

60 to 120.

• Macro-mixing length was not able to be determined visually due to low coloration of the bulk stream.

Case 1 2 3 4 5 6 7

𝑓 (Hz) 0 1.5 1 1 0.5 1 1.5

𝑥

𝑜

(mm) 0 2.8 4.24 6.36 12.68 12.68 12.68

𝑅𝑒

𝑜

0 395 398 598 596 1191 1787

𝑋

𝑠

0.38 0.36 0.35 0.30 0.05 0.10 0.22

Macro-mixing length

(# baffle cell) Not reached Not reached 21 20 4 6 14

References

[1] Stephens G.G., Mackley M.R., (2002), Exp. Therm. Fluid Sci., 25: 583 - 594.

[2] Mazubert A., Crockatt M., Poux M., Aubin J., Roelands M., (2015), Chem. Eng. Technol., 38: 2161 - 2169.

[3] Lawton S., Steele G., Shering P., Zhao L., Laird I., Ni X.W., (2009), Org. Process Res. Dev., 13: 1357 - 1363.

[4] Hewgill M.R., Mackley M.R., Pandit A.B., Pannu S.S., (1993), Chem. Eng. Sci., 48: 799 - 809.

[5] Lobry E., Lasuye T., Gourdon C., Xuereb C., (2014), Chem. Eng. J., 259: 505 - 518.

[6] Fournier M.C., Falk L., Villermaux J., (1996), Chem. Eng. Sci., 51: 5053 - 5064.

[7] Guichardon P., Falk L., (2000), Chem. Eng. Sci., 55: 4233 - 4243.

[8] Panié S., Loebbecke S., Tuercke T., Antes J., Bošković D., (2004), Chem. Eng. J., 101: 409 - 419

Conclusions

• Mixing length and 𝑋

𝑠

is directly proportional to 𝑥

𝑂

and inversely proportional to 𝑓 , and not only dependent of the mixing intensity 𝑅𝑒

𝑜

.

• The influence of 𝑥

𝑂

and 𝑓 on the micromixing efficiency in non-negligible when a reactive side stream is added by a tee injection before the first baffled cell.

Future work

• Identify the relationship between 𝑋

𝑠

and oscillatory and geometrical parameters:

– Experiments with higher 𝑥

𝑂

Τ 𝑙

𝑏

values.

– Study the influence of higher 𝑅𝑒

net

by increasing the main flow rate.

• The influence of geometry and new configurations will be studied to improve the micromixing performance in the COBR.

• Sensitivity problem.

– Acid concentration of 0.03 𝑀: 𝑋

𝑠

only varied slightly or not at all with the oscillatory conditions.

– Acid concentration of 0.015 𝑀 was used in further experiments.

• Presence of oscillations leads to a decrease in the 𝑋

𝑠

values.

• Segregation index is not solely correlated with 𝑅𝑒

𝑜

.

• Constant 𝑓: an increase in 𝑥

𝑂

decreases mixing length and 𝑋

𝑠

.

• Constant 𝑥

𝑂

: an increase in 𝑓, decreases mixing performance, and leads to longer mixing lengths.

• High 𝑥

𝑂

and low 𝑓 detaches the acid stream from the reactor wall, allowing it to be

engulfed by the bulk stream at shorter lengths.

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