Crystallization of α-glycine by anti-solvent assisted by ultrasound

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Submitted on 23 Apr 2018

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Crystallization of α-glycine by anti-solvent assisted by ultrasound

Hector Rodriguez Vera, Fabien Baillon, Philippe Accart, Fabienne Espitalier, Olivier Louisnard

To cite this version:

Hector Rodriguez Vera, Fabien Baillon, Philippe Accart, Fabienne Espitalier, Olivier Louisnard. Crys-tallization of α-glycine by anti-solvent assisted by ultrasound. 16th Meeting of European Society of Sonochemistry (ESS16), Apr 2018, Besançon, France. �hal-01773871�

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Crystallization of

α

-glycine by anti-solvent

assisted by ultrasound

Hector Uriel Rodriguez Vera, Fabien Baillon,

Philippe Accart, Fabienne Espitalier, Olivier Louisnard

Introduction

I

Ultrasound and Crystallization by cooling:

Reduction of the induction time and a reduction of the size of the formed crystals with equivalent

supersaturation.

I

Ultrasound and Crystallization by anti-solvent effect:

Do ultrasound have an influence on the crystallization of

glycine by antisolvent effect in batch system (induction time, crystal size distribution, polymorphism)?

Materials and methods

I

Glycine

• 3 polymorphic:

α

,

β

and

γ

(stable)

• Initial solid:

α

(mass purity

99.9%) • Soluble in water • Insoluble in ethanol

I

Analyzes • Refractive index • MEB • Laser granulometry

• Dissipated power measured in water Bioblock generator, 20 kHz Peristaltic pump Temperature probe Tsolution Peristaltic pump ethanol

Previous work without US

I

Experiments without ultrasound (reference)

• 4 flow rates (g.min−1_{) of ethanol}

• Supersaturation ratio

S

=

_C C

eq(T,R)

Results: effects of ultrasound

I

Influence of US power, for constant flow rate

I

Influence of the pulsation frequency

Maximal supersaturation and induction time

28 100% 13.4 75% 11.2 50% 8.1 25% 0

US power, P (W) and Pulsed mode (%) 1 1.02 1.04 1.06 1.08 1.1 1.12 1.14 1.16 Super saturation ratio, S (-) 0 5 10 15 20 25 30 35 40 Indu ction time, t ind (min)

US in pulsed mode: equivalent results in terms of size

and concentration profile

I

Influence of the ultrasonic power

I

_{Influence of ethanol flow rate}

Maximal supersaturation and induction time

US 28 W US 28 W US 28 W US 28 W US 28 W US 28 W US 28 W US 28 W 0.046 0.090 0.190 0.360

ethanol flow rate (g.min-1) 1 1.02 1.04 1.06 1.08 1.1 1.12 1.14 Super saturation ratio, S (-) 0 20 40 60 80 100 Indu ction time, t ind (min)

Conclusions and perspectives

I

Trends with US vs. without US:

• Smaller crystals, monomodal size distributions • Decrease of induction time

• The

α

-form is obtained with and without ultrasound

• Equilibrium concentration more quickly reached (S

7→

1)

I

Work in pulsed mode (> 25%):

identical results in continuous mode

I

Transpose in continuous mode:

SONOCRISTAL® (prototype developed in collaboration with SYNETUDE SAS)

16th _{Meeting of European Society of Sonochemistry (ESS16), Besançon (France), April, 15-19, 2018}

Université de Toulouse,

IMT Mines Albi, Centre RAPSODEE, UMR CNRS 5302 Campus Jarlard, 81013 Albi France _References Yang, X., Ching, C. B., Wang, X. J. & Lu, J.,

2006, AICHE annual meeting, San Fransisco, CA. El Bazi, W., 2011, thèse du Conservatoire national des Arts et Métiers.

Louhikultanen, M., Karjalainen, M., Rantanen, J., Huhtanen, M. & Kallas, 2006, J. International Journal of Pharmaceutics, 320, 23–29. Baillon, F., Espitalier F., Cogné C., Peczalski R., Louisnard O., 2014. Power ultrasonics: Applications of high intensity ultrasound, 845-874, Eds: Juan A. Gallego-Juárez and Karl F. Graff. Woodhead Publishing. Q _Contacts Fabienne.Espitalier @mines-albi.fr Fabien.Baillon @mines-albi.fr