Photo-optical In-situ Measurement of Drop Size ...projet.ifpen.fr/Projet/upload/docs/application/pdf/2016-10/4._pancko… · -optical In situ Measurement of Drop Size Distributions:

Photo-optical In-situ Measurement of Drop Size Distributions: Application in Research and Industry

Robert P. PANCKOW1,4, Laura REINECKE2, Maria C. CUELLAR3, Sebastian MAAß1

1Technische Universität Berlin, Fachgebiet Verfahrenstechnik, Berlin, Germany; 2Franken Filtertechnik KG, Hürth, Germany; 3TU Delft, Department of Biotechnology, Bioprocess Engineering, Delft, Netherlands; 1SOPAT

GmbH, Berlin, Germany

Dynamics of Evolving Fluid Interfaces – DEFI, IFPEN/Solaize - France, 12-13 October 2016

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Agenda

Drop size measurements in fermentation broth

Separation efficiency of a droplet separator with/without plate internals

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Microbial production of diesel and jet fuels

investigates cost reduction by integrating fermentation and product recovery. Partners:

Engineering of microorganisms (yeast, bacteria) to produce diesel and jet fuel replacements (e.g. trans-β-Farnesene by Amyris)

Amyris’ Farnesene production plant in Brazil

(source: Amyris)

Formation of oil-in-water emulsions during fermentation

Delft Advanced Biorenewables

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Control of separation efficiency

Removal of droplets in emulsions, cut-off size varies according to user requirements

Application in biodiesel, glycerol treatment, plastics, chemical, oil & gas upstream processes…

Large number of influencing parameters: physical system, Q, σ, μ, Δρ, ϕv, dispersion direction, inlet droplet population, internals/no internals…

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Adjustable probe length

Micro Flow Cell (MFC)

SOPAT probes (1 – 10000 µm)

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Image Analysis: Function Overview

-

?

K

*

d32

n

∑ n Images

Manual counting

Pattern-Matching

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Results – Fermentation

Evaluation of effect of individual medium components on oil droplet coalescence by use of SOPAT probe

Example of pictures taken with the SOPAT probe

Heeres et al. 2015. Biotechnology Journal 10:1206-1215.

1200 rpm 600 rpm

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Monitoring of Sauter diameter

Heeres et al. 2015. Biotechnology Journal 10:1206-1215.

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Drop size distribution

e06 (200 µm gap), e05 (1 mm gap) a) density distribution q0 of number

b) cumulative distribution Q3 of volume

Adjustable flow gap for in-situ measurement

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Conclusions – Fermentation The photo-optical measuring method detects a broad range of droplet sizes and allows

differentiation from other dispersed components such as microbial cells and bubbles In the model mixture tested, the SMD d3,2 ranged between 80 and 100 μm, while in

current fermentations in biofuel production mean droplet sizes are in the range of 10 μm

Ongoing research focuses on strategies for promoting droplet coalescence and avoiding

droplet stabilization during fermentation.

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Results: Droplet separator Purpose: Optimization of separation efficiency by use of plate pack internals with

different gaps

Laboratory plant separator, D = 100 mm, L = 400 mm; with/without plate internals; DSD at inlet adjustable in range 1…1000 microns; continuous phase: tap water; dispersed phase 1) silicon oil, 2) paraffin oil

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outlet, no internals inlet

outlet, with internals inlet

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Influence of dispersed phase

ϕd=1 vol.-% ca. 20000 droplets

ϕd=1 vol.-% ca. 20000 droplets

Significant influence of density difference

density viscosity

kg m-3 mPas

Silicon oil 920 5.09

Paraffin oil 760 1.46

Water 998 1

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Influence of internals

ϕd=5 vol.-% Silicon oil/water 7 mm plate gap

ϕd=5 vol.-% Silicon oil/water 7 mm plate gap

Separation efficiency [SOPAT]

Separation efficiency [volumetric]

Vol.-% Vol.-%

Without plates 68 69

With plates 95 95

Significant impact of plate internals on the separation efficiency

In-situ probe showed very good agree-ment with volumetric measurements

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Conclusion

Inline particle size measurement technology is suitable for fermentation and separation applications, amongst others

The SOPAT software is able to distinguish between different dispersed phases, such as disturbing bubbles and dirt particles

As the results are available inline and in real-time, a closed control loop can be established in the future

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Attachments

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Impact

[1] Dittler, I., Kaiser, S., Rojahn, J., Kraume, M., Eibl, D., 2014. A cost-effective and reliable method to predict mechanical stress in single-use and standard pumps, Engineering in Life Science, 14: 311–317 [2] Panckow, R., Maaß, S., Emmerich, J. und Kraume, M., 2013. Automated Quantification of Bubble Size Distributions in an Agitated Air/Water System, Chemie Inge-nieur Technik, 85(7): 1036-1045. [3] Schilder, L., Maaß, S. und Jess, A., 2013. Effective and Intrinsic Kinetics of Liquid-Phase Isobutane/2-Butene Alkylation Catalyzed by Chloroaluminate Ionic Liquids. Industrial & Engineering Chemistry Research, 52(5): 1877-1885. [4] Maaß, S., Rojahn, J., Hänsch, R. und Kraume, M., 2012. Automated drop detection us-ing image analysis for online particle size monitoring in multiphase systems. Computers and Chemical Engineering, 45: 27-37. [5] Maaß, S. und Kraume, M., 2012. Prozesse auf Basis der Partikelgröße steuern. CIT Plus, 6 (ISSN 1436-2597): 31-33. [6] Maaß, S., Paul, N. und Kraume, M., 2012. Influence of the dispersed phase fraction on experimental and predicted drop size distributions in breakage dominated stirred liq-uid-liquid systems. Chemical Engineering Science, 76: 140-153. [7] Maaß, S., Buscher, S., Hermann, S. und Kraume, M., 2011. Analysis of particle strain in stirred bioreactors by drop breakage investigations, Biotechnology Journal, 6(8): 979-992. [8] Maaß, S., Rehm, T. und Kraume, M., 2011. Prediction of drop sizes for liquid-liquid systems in stirred slim reactors - Part II: Multi stage impellers, Chemical Engineering Journal, 168(2): 827–838. [9] Maaß, S., Wollny, S., Voigt, A. und Kraume, M., 2011. Experimental comparison of measurement techniques for drop size distributions in liquid/liquid dispersions, Ex-periments in Fluids, 50(2): 259-269. [10] Maaß, S., Metz, F., Rehm, T. und Kraume, M., 2010. Prediction of drop sizes for liquid-liquid systems in stirred slim reactors - Part I: Single stage impellers, Chemical Engi-neering Journal, 162(2): 792-801. ….

• More than 40 publications • More than 100 oral and poster presentations at conferences

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Comparing Inlet-Outlet: Separation Efficiency

Measured DSD for the gap size 1.5 mm at the inlet and outlet for V̇ = 100 L h-1, φd = 1 vol%

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outlet inlet

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Selection and optimization of separation method requires DSD information

• DSD is influenced by broth composition, reactor parameters, oil fraction, fermentation age,…

• Off-line DSD measurement methods are not suitable (e.g. due to non homogeneous sampling, change in DSD during sample procedure, aging of sample)

• Challenges for in-situ measurement: presence of other phases (gas bubbles, microorganisms), technical limitations (e.g. sterility).

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Measurement Technique

Workstation (optional: communication with PCS)

+

max. 4 m

m

ax. 70m (Cat 7)

Central Box

Probe

Measurement range of photo-optical SOPAT probes

1µm 1mm 100µm 10µm 10mm

microscopic

mesoscopic

macroscopic

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Image Analysis: Pattern-Matching

Example template represents the ideal

particle for every size class

Q(x,y)

T Manual pre-selection of individual

particle examples

Feature-extraction

Template „T“ is created

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Adjustable flow gap for in-situ measurement

1µm 1mm 100µm 10µm 10mm

SOPAT probes Probes for microscopic range

Cell organisms (algae, yeast) Powders Nucleation processes ...

Illumination by transmission

Diapositive numéro 1AgendaMicrobial production of diesel and jet fuelsControl of separation efficiencySOPAT probes (1 – 10000 µm)Image Analysis: Function OverviewResults – FermentationMonitoring of Sauter diameterDrop size distributionConclusions – FermentationResults: Droplet separatorDiapositive numéro 12Influence of dispersed phaseInfluence of internalsConclusion AttachmentsImpactComparing Inlet-Outlet: Separation EfficiencyDiapositive numéro 19Selection and optimization of separation method requires DSD informationMeasurement TechniqueImage Analysis: Pattern-MatchingSOPAT probes

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Photo-optical In-situ Measurement of Drop Size ...projet.ifpen.fr/Projet/upload/docs/application/pdf/2016-10/4._pancko… · -optical In situ Measurement of Drop Size Distributions: