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HAL Id: hal-02097218

https://hal.archives-ouvertes.fr/hal-02097218

Submitted on 5 Jun 2020

HAL is a multi-disciplinary open access archive for the deposit and dissemination of sci- entific research documents, whether they are pub- lished or not. The documents may come from teaching and research institutions in France or

L’archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d’enseignement et de recherche français ou étrangers, des laboratoires

Drying research From physical and biological mechanisms to breakthrough innovation

Luca Lanotte, Romain Jeantet

To cite this version:

Luca Lanotte, Romain Jeantet. Drying research From physical and biological mechanisms to break- through innovation. STLOpendays, Institut National de Recherche Agronomique (INRA). UMR UMR INRA / AgroCampus Rennes : Science et Technologie du Lait et de l’?uf (1253)., Mar 2019, Rennes, France. �hal-02097218�

(2)

STLOpen Days 19-21 March 2019

Drying research

From physical and biological mechanisms to breakthrough innovation

Luca Lanotte & Romain Jeantet

(3)

Dairy

liquid Concentrate Crystallised

concentrate Powder

6-10% w/w 50 - 60% w/w Heat treatment

Membrane separation Vacuum evaporation

Lactose crystallization

Spray drying

Storage

95-98%

w/w

Recombined dairy liquid

Rehydration

Functional & nutritional properties

Concentration, drying and rehydration of dairy products

Drying research

(4)

Context , Research topics , Strategy

q Massive growth of Infant milk formula (IMF) / protein isolate market

q Controlled properties, incorporation of live probiotics

q Environmental and costs concern Understand the particle

formation mechanisms Identify the key parameters that rule the powder properties and evolution

Explore new technological concepts for technological breakthrough innovation

Consider simplified &

controlled models (dairy

colloids, bacteria)

Observe the phenomenon

at different scales to make

the study possible

Combine disciplines:

from biology to soft matter and

chemical engineering

Partnership to feed the scientific

questions and identify technological

outputs

(5)

1.

Exploring particle formation to control IMF properties

2.

Triggering the protection mechanisms to maximize survival of bacteria

3.

Redesigning the process for the

production of whey/permeate powders

(6)

Coupling methods

Single droplet 3D / 2D

Mono-disperse droplets Spraying cone

of droplets Milk colloids

PARTICLES PROPERTIES

§ Controldrying history

§ Get homogenous samples

§ Analyzephysical properties

SCALE UP

§ Validateon an industrial scale

§ Control

PARTICLE FORMATION

§ Control and study the drying kinetics

§ Record in situ deformation

§ Whey protein (WP)

§ Micellar casein (MC)

§ Single or mixed together

Strategy - Study of the drying process on multi-scales

§ Mass balance

§ Microscopy

§ Rheology

(7)

1. Homogeneous kinetics &

shrinkage

2. Skin formation:

sol/gel transition

3. Mechanical stress

= f (properties)

Brittle (WP)

Ductile (MC)

Powder properties

Specific signatures of WP and MC proteins governing the particle formation / shape and properties, regardless of

the drying kinetics

Langmuir29(2013) 15606 - 15613 Drying Technol32(2014) 1540 - 1551 Food Hydrocolloids48(2015) 8 - 16 Food Hydrocolloids52(2016) 161 -166

Protein signature in the course of drying

Micellar Casein

Whey Protein

(8)

WP 60-40

MC 20-80

60-40 WP

MC 20-80

Single pendant droplet

Scanning Electron Microscopy (SEM)

Flying monodisperse droplets

Optical Microscopy

Protein signature : the case of protein mixes

In this case of protein mixes, the major protein rules the transition and final shape

of the droplet / particle

(9)

OUT

IN

Colloids and Surfaces A 553(2018) 20 -27

Is the skin composition representative of the

bulk? Calcium (Ca)

S

IGNATURE OF

MC

Elemental analysis by SEM (EDS)

Over-representation of WP on the external part of the dry skin in WP/MC mixes: how

to explain such behavior?

(10)

Understanding the drying mechanisms in colloidal

polydisperse systems Control of the nutritional

properties of the powders (rehydration)

FILM FORMATION IN BINARY COLLOIDAL MIXTURES

Zhou J. et al., PRL 118, 108002 (2017).

Fortini A. et al., PRL 116, 118301 (2016).

Small on top theory

Due to osmotic pressure, smaller colloids accumulate on the external part of the skin/gelled

layer passing through its interstitial pores

Characterization of the sol-gel transition in dairy mixes

Drying-induced colloid behavior

(11)

2.

Triggering the protection mechanisms

to maximize survival of bacteria

(12)

Resistant strain selection,

Cross-protection via sublethal stresses, etc.

Protective food grade constituents:

Carbohydrates, proteins, polymers, minerals

Optimize/moderate drying conditions:

multistage, belt, etc.

Stirring

Coupling strategies to improve probiotics viability?

Strategies in probiotics drying research

(13)

A coupled approach for a novel process

Probiotics Growth medium

Sterilization

Growth

Separation Rinse

Bacterial paste

Drying medium

Sterilization

Re-suspension

Pumping Spray drying

Stirring

Cross-protection Sublethal osmotic

Food grade materials Carbohydrates

Proteins Polymers

Minerals

Multi-stage drying Pre-concentration

Concentrated 2-in-1 (Growth

& Drying) Medium

Stress Tolerance Lower q / Energy savings

(14)

0%

20%

40%

60%

80%

100%

120%

5 10 20 30 40

Survival %

Heat

60°C/10 min

0,008% 0,356% 0,022%

0%

5%

10%

15%

20%

25%

30%

35%

5 10 20 30 40

Survival %

AcidpH 2/1h

0,005% 0,006%

0,0%

0,5%

1,0%

1,5%

2,0%

2,5%

5 10 20 30 40

Survival %

Bile-salt

0.1% / 1h

30SW Protein upregulation

(Label-free proteomics):

Osmoregulation

Glycine betaine transporter

Stress tolerance

Chaperone, Cysteine synthase

Osmoregulation induce protection mechanisms before drying

30 SW L. casei growth

App Env Microbiol 82 (2016) 4641 - 4651

5SW

Accumulation

Polyphosphates

Glycogen (energy for long term survival)

Trehalose (involved in anhydrobiosis)

+

Multi-stress resistant phenotype Osmoregulation

Optimal content

(15)

5%or 30% sweet whey

Sterilization

Inoculation of bacteria

Growth

Bacterial culture

Lab-scale

140 °C

60 °C Powder 1

140 °C

60 °C 47 °C

Powder 4

Multi-stage

Sieve

Fluid-bed Drying

Belt Drying Powder 3

Sieve

Single stage

1~2 L fermentation

~3 kg/h drying

Drying bacteria at different scales

Powder 2

127 °C

(16)

30% SW growth results in sharp

survival rate increase Scale-up feasibility

Bacteria survival upon drying

J Food Eng 196 (2017) 11 - 17

Acquired cross protection with multi stage scheme provides 100% survival ð Patented process EP 15 306465.4 - 1357

(17)

3.

Redesigning the process for the

production of whey/permeate powders

(18)

concentrate DM, but limiting viscosity / pumping and spraying

Current bottlenecks in whey/permeate powder production

Spray drying 60 > 97% DM Concentration

6 > 60 % DM Batch

crystallization

Whey or permeate

powder

Liquid whey or permeate

Falling-film

evaporators Multi stage

dryer

SEC (kJ.kg-1

water) 418 kJ.kg-1

x 10

5256 kJ.kg-1

55% of the overall energy for

# 4% of the water removed

Innovative process PST based on thin-film rotary evaporator where viscosity is controlled by a vigorous mechanical treatment

that maintains a fluid flowing state at high DM

(19)

PST: a new process for whey/permeate powder production

Spray drying 60 – 97% DM Concentration

6 > 60 % DM Batch

crystallization

Whey or permeate

powder

Liquid whey or permeate

Falling-film evaporator

Over concentration 60 > 80 % DM

2 Thin-film horizontal rotary evaporators

Granulation

Final drying 88 > 97 % DM

16 t 1,6 t

1,2 t

2,4 t

1,2 t 1,2 t

Whey or permeate

powder q Feasibility of PST at pilot scale ?

q Properties of the resulting powder / standard?

q Resulting energy savings?

(20)

Similar powder characteristics, lower energy requirements

q Non significantly different features of PST powder compared to control

q PST process was run successfully for long duration experiments > 6 hours

0 100 200 300 400 500

0 400 800 1200 1600 2000

Bulk density

(kg.m-3) true density (kg.m-3)

d10(µm) d50 d90 solubility

(%)

dispersibility (% w/w)

0 50 100

q PST process significantly saves energy compared to the standard drying process

q Estimation of energy costs on the sole basis of the energy required for removal of water

q Drying step (60 to 97 % DM): 32% energy savings

q Whole process (6 to 97 % DM): 11% energy savings

(21)

PST process in short

VALIDATION

• Feasibility of PST process at pilot scale / long duration for the production of permeate powder

• Satisfactory properties of the resulting powder

INNOVATION

• Potential new products …

• Produced in a sustainable way…

• Using breakthrough innovation REDUCTION

• Energy savings estimation range from 10 to 30%

• Building savings estimated at 40%

• Water, CIP solutions and waste volumes should be cut as well

(22)

Conclusion and perspectives

Extensive work on IMF formulation is needed

Determines nutritional properties

Conditions particle intrinsic features, then powder properties

Enhances probiotics survival during drying and in the dry state

Research strategy to overcome industry challenges

Needs to address growing market bottlenecks / societal issues

Identifying the mechanisms at small scale, scale up needed

Multidisciplinary approach is mandatory: physics / biology / medical

Next step in IMF research / development

Understand the mechanisms governing the skin formation in colloid mixes

Better control the end use properties while considering real complex formula in single drop experiments

(23)

THANK YOU FOR YOUR ATTENTION

MERCI

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