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ENITIAA, BP82225, F-44322 Nantes - Email : [email protected] Microencapsulation ? Denis Poncelet

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Page 1: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Microencapsulation ?Denis Poncelet

Page 2: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Introduction : définitions

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

microcapsulesmicroparticlesmicrospheres

nanocapsulesnanoparticlesnanosphères

micellesliposomes

(micro)emulsions

molecular inclusion

matrixmicrocapsule

reservoir or hollowmicrocapsule

polynuclear or multicore

microcapsule

micelle

uni- or multilamellar vesicle

Hydrogel bead

Page 3: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Immobilization

Continuous processing (bio-cells & enzymes)

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

Volatile compounds

Lactic bacteria culture

free cells< 108

cells/ml

immobilized> 1010cells/ml

http://www.mane.com/

Page 4: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Protection

About degradation (O2, ligth, heat, water)

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

During shell-life, processing and digestion

www.customprobiotics.com

Vitamin A / monosodium glutamateappearance (white)protection (water, T, ligth)

www.encap.com

www.balchem.com

Meatshure

Page 5: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Protection

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

Taste masking

Medium protection

Ferrous fumarate agglomerated and coated with 60% hydrogenated soy oil using the Wurster process. 100-450 µm

Immunoprotection

www.human-nutrition.basf.com

http://www.islet.com

Page 6: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Release

Diffusion-rehydration-degradation-rupture

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

Chemical - physical - mechanical factors

www.salvona.com

Page 7: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Release of a by-product

Water

2 enzymesglucose+ HCN

lactoperoxidase system (LPS)

OSCN- Listeriabactericide

Objectives : Release

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

material immobilizationcontrol of hygroscopyflowdability & dispersibilityenzyme protectionhigh reaction efficiencycontrolled releaselong term & more efficient action against listeria

Page 8: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Structuration

Liquid or gaz to solid

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

Dispersibility

Solubility

Flowdability

Tabletisatisable

Dust free powder

Hygroscopicity controle

Spic and Span

Page 9: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Objectives : Structuration

Microencapsulation

Entrapment of a material inside microparticles for :

immobilized itprotect itrelease itstructure it

Visual aspect and marketing concept

http://www.colorcon.com

http://www.coletica.fr

http://euracli.fr/

Page 10: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Microencapsulation : Applications

Chemistry Printing & recording Carbonless paper Adhesives Pigments and fillers Catalysts

Agriculture Fungicide - herbicide Insect repellent Biopesticide Pigments and fillers Artificial insemination

Food & feed Aromas Probiotics Unsaturated oil Enzyme food processing aminoacid for cows

Medecine & Pharmacy & vetinary Controle release Taste masking Vectorisation Artificial organs single dose treament

Biotechnology & enviroment Continuous reactor Shear protection Reactor oxygenation Bioprobes

Consumer & diversified cosmetics detergents (enzymes) sanitary (active, aromas)

Page 11: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

0

200

400

600

800

1000

1200

1400

1600

1800

2000

Num

ber o

f doc

umen

ts

1965

1967

1969

1971

1973

1975

1977

1979

1981

1983

1985

1987

1989

1991

1993

1995

1997

1999

2001

2003

Year

Non-patent (7500)

Patent (11000)

non patents (7500)

patents (11000)

2000

1500

1000

500

01965 1970 1975 1980 1985 1990 1995 2000

From Bojana boh (2003) MLL vol. 6, Citus Book, london, UK.

Microencapsulation documents referenced in Chemical Abstracts

Microencapsulation : Applications

Page 12: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Encapsulation : methods & technologies

Incorporation du principe actif

liquid in air liquid in liquid

PrillingSpraying

Emulsion

Dispersion

StabilisationSolidification Gelification

PolymerisationCoacervation

Liquide(solution, melting, emulsion, suspension)

Solide

Technics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

Evaporation (drying)Solidification Evaporation

Coalescence

1

2

3

1 5Microemulsion

2 3 4

Chemistry Physicochemistry Physic

Step

Page 13: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Prilling / dropping methods

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

0-10 kV

Rezonnance Nozzle T.

Jet cutter Electrostaticgenerator

Rotative or spinning disk

liquid in air

Page 14: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

http://www.nisco.ch

Prilling / Electrostatic generator

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

0-10 kV

low dispersion (20 %)50 to 1000 micrometerslarge range of viscosity viscositylow troughput (10 to 100 ml/h)

U

liquid in air

Page 15: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Prilling / Rezonnance Nozzle Technology

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

low dispersion (5-10 %)high troughput (0.1 to 2 l/h)100 to 1000 micrometersincluding medical applicationslow viscosity

http://www.inotech.ch

liquid in air

Page 16: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Prilling / Jet cutter

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

low dispersion (5-10 %)high troughput (0.1 to 5 l/h)300 to 1000 micrometershigh viscosity

http://geniaLab.de

pectate beads with TiO2 and vitamine, Ø 500 µm

liquid in air

Page 17: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

www.swri.org

Particle and coating technologywww.pctincusa.com

Prilling / Rotating devices

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

www.niro.com

liquid in air

Page 18: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Prilling / Stabilisation

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

GelificationCoacervation

Liquide

Evaporation

Gel

Gelation bath

Melted material

Coldair or water

polymer+ solvent

Hot air

Polymer-

Polymer+

Solidification

Gelification

InterfacialCoacervation

Evaporation or drying

liquid in air

inner core = solution, emulsion, suspension, powder

Page 19: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Prilling / Coextrusion

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

GelificationCoacervation

Liquide

Evaporation

liquid in air

http://www.inotech.ch

Page 20: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Spraying / Stabilisation

Principe actif

Pulvérisation

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

http://www.niroinc.com/

Page 21: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Pulverisation / stabilisation

Principe actif

Pulverization

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

Spray dryingspray = aqueous solutionhot air

! over heating! low initial dry matter! matrix structuration

Spray chillingspray = thermogelcold air + drying air

Spray cooling or congealingspray = hot meltcold air> high yield, fast process

Spray = solution, emulsion, suspension

http://www.nutriprocess.com/

http://www.innov-ia.com/

Page 22: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

membrane formingmaterial + cells

Cross-linkerVegetable ormineral oil

static mixers

Batch processTurbine reactor

Continous processStaticmixers

Emulsion / dispersion

Principe actif

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

liquid in liquid

Emulsion Microemulsion

fast dispersion (< 1 sec)high troughput (m3/h)Cheap, easy

Page 23: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Acid dichloride(Poly)amine

Oil

(Interfacial)Polymerisation

Solvent

water

Polymer + solvent

Solvent evaporation or extraction

Acid or salt

Polymer(s) solution

Oil

Coacervation

Alginate +CaCO3

Aceticacid

Vegetal Oil

Internal gelationPrincipe actif

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

liquid in liquid

Emulsion Microemulsion

K-carraghenane

Vegetal Oil

Thermal gelation

Emulsion / stabilisation

inner core = solution, emulsion, suspension, powder

Page 24: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Principe actif

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

liquid in liquid

Emulsion Microemulsion

nanoencapsulation

surfactant

Nanoencapsulation & molecular inclusion

Liposomes

molecular inclusion

Page 25: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Coating - pelletizing - layering

Principe actif

Solide

Technics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

SolidificationEvaporation

Coalescencehttp://www.glatt.dewww.encap.com

Page 26: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Fluid bed technologies

Principe actif

SolideTechnics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

Solidification

Evaporation

Coalescence

http://www.glatt.de

Rotor sprayvery dense coating

spheronisationlow drying capacity

lower cooling capacity

Top spray Coating & DryingHot melt coatingAgglomerationHigh capacitypoor coating

WursterCoating & Dryinglower capacity

more homogeneous coating

Page 27: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Advances coating technologies

Principe actif

SolideTechnics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

SolidificationEvaporation

Coalescence

Pan coaterCoating & agglomeration

dry powder coatinglarge particleslower capacity

Continuous coaterlower cost

higher capacity

Spouted bedbetter particle circulation

better temperature controle

T<

Page 28: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

Coating / stabilisation processes

Principe actif

SolideTechnics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

SolidificationEvaporation

Coalescence

Evaporation (spray coating)spray = solutionhot air! slow process! energy demand

Coalescence (dry powder coating)spray = fine powder + plastifiantair at room temperature

Spray = solution, emulsion, suspension, powderpolymer, filler, surfactant, active

Solidification (hot melt coating)spray = hot meltcold air air

http://mcc-ch.org

www.syntapharm.com

Page 29: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

1000 groupsover 80 countries(30 % industrials)

research coordination over 25 (-> 35) countries

Topical team to develop research projects

European plateform for promoting encapsulation industrial business

Marie Curie thematicnetwork

UNESCO/INTAS network

Fluid bed technologies

http://bioencapsulation.net

http://ncapsolutions.com

http://COST865.bioencapsulation.net

865

Page 30: Denis Poncelet -  · PDF fileDenis Poncelet. ENITIAA, BP82225, F-44322 Nantes ... Prilling Spraying Emulsion Dispersion Stabilisation Solidification Gelification Polymerisation

ENITIAA, BP82225, F-44322 Nantes - Email : [email protected]

http://bioencapsulation.net/XIII_IWB http://bioncap.com