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ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

Microencapsulation ?Denis Poncelet

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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/

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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/

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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)

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

0

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Year

Non-patent (7500)

Patent (11000)

non patents (7500)

patents (11000)

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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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

Prilling / Coextrusion

Principe actif

Prilling Spraying

Dispersion

StabilisationSolidification

GelificationCoacervation

Liquide

Evaporation

liquid in air

http://www.inotech.ch

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

Spraying / Stabilisation

Principe actif

Pulvérisation

Prilling Spraying

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

http://www.niroinc.com/

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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/

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

Principe actif

Dispersion

StabilisationSolidification

Gelification

Polymerisation

Coacervation

Liquide

Evaporation

liquid in liquid

Emulsion Microemulsion

nanoencapsulation

surfactant

Nanoencapsulation & molecular inclusion

Liposomes

molecular inclusion

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

Coating - pelletizing - layering

Principe actif

Solide

Technics

Coating / agglomeration

Pan reactor / Fluid bed

Stabilisation

SolidificationEvaporation

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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<

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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

ENITIAA, BP82225, F-44322 Nantes - Email : poncelet@enitiaa-nantes.fr

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