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Titel van de presentatie 14-11-2014 10:52
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Coating Technology and Encapsulation – Closely Connected
dr. ir. Nicole Papen-Botterhuis, Scientist
TNO Materials Solutions
Eindhoven
Encapsulation Technologies – Characteristics
High performance materials as well as processing technologies are
required to meet the product demands
Properties:
Size (macro, micro, nano)
Size distribution (monodisperse, polydisperse, bimodal)
Morphology (matrix, core-shell, multicore-shell, double walled, sandwich)
Loading efficiency (maximize active vs. encapsulation material)
Encapsulation efficiency (minimize loss of active material)
Nicole Papen-Botterhuis
TNO Encapsulation Team
barrier
release release
barrier
release Core-shell Matrix Sandwich
Titel van de presentatie 14-11-2014 10:52
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Encapsulation – Why?
Protect ingredients
(against oxygen, water)
Separate components,
prevent interaction
Nicole Papen-Botterhuis
TNO Encapsulation Team
Controlled
release
Adjust
properties
Keep
outside
out
Keep
ingredient
inside
Delayed/slow: Prevent
burst release / premature
leaching (drugs, nutrients
antimicrobials, fertilizers)
Triggered: pH, water,
temperature, enzymes,
pressure/force
Easy & safe handling (solid vs.
liquid, decreased volatility)
Enzyme immobilization
Taste masking
Biocompatibility
Change physical properties
(solubility, structure, density)
Flowability
Hygroscopic control
Microencapsulation can bring you new products, new functionalities,
better product properties, higher added value – if done right
Coating Technology and Encapsulation – Closely Connected?
Encapsulation is in fact the coating of particles at the micro/nanoscale
Different processes/materials
What can we learn from each other?
Capsules can be applied in coatings to obtain an added value or
functional coatings
Isolation
Self-healing
Controlled release of active ingredients such as biocides
Stabilization of pigments
Sometimes added value can also we obtained without capsules, if the
barrier value of the coating itself can be adjusted.
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Development of encapsulation technologies
BASE TECHNOLOGY Year ADDITION Controlled Release
Spray Drying of Solids 1872 Emulsified Oils, 1925,
Special Disk, 1949,1987 Spray Dried Flavors,
Reservoir Structure
Extrusion of Synthetic
Fibers into a bath 1920 Flavor Oils, 1957 Sunkist Process
Fluid Bed Drying Top, Side, Bottom Spray
Nozzle & Partition 1965 Wurster Coating,
Agglomerization
Emulsion polymerization Add Oil to Polymer APS Polytrap
Spun Sugar (Cotton Candy) Emulsify Oil into Hotmelt Fuisz 1991
Droplet Stabilization With
Surfactants Form a Massive Wall Coacervation 1951
Parylene Coating Tumbling of Powder Parylene μE 1983
Polycondensation of Nylon >1930’s Water Medium Interfacial
Polymerization
U/F Resins <1920 Coacervation Formation Polymethyleneurea, U/F
Pan Coating 19th
Century Specialty Coating, e.g.
enteric, “tunnel coating” Enhanced Release,
continuous process
Nicole Papen-Botterhuis
TNO Encapsulation Team
Ronald Versic, RT Dodge Company, USA
Ron Neufeld, Queen’s University, Canada
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Common microencapsulation technologies
Technology Matrix or
Core-shell?
Size
(distribution)
Cost Production
Use
Spray drying large variations
2 - 100 µm
low continuous +++
Spray chilling 20- 200µm low continuous +++
Extrusion > 50 µm low continuous ++
Pan coating >500 µm low batchwise ++
Fluidized bed >50 µm medium batchwise
/continuous
++
Coacervation 1 - 500 µm
high batchwise ++
Interfacial/ in situ
polymerization
1 - 500 µm high batchwise +
Nicole Papen-Botterhuis
TNO Encapsulation Team
LOW
COST
HIGH
COST
Nicole Papen-Botterhuis
TNO Encapsulation Team
Adjusted from www.SWRI.org
Titel van de presentatie 14-11-2014 10:52
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Spray-drying
Widely used in food industry, e.g. to:
convert liquids into powders
protect flavour oils or other ingredients against degradation
Typically aqueous formulations of shell / matrix material
Ingredient either dissolved in matrix or present as emulsion (multi-core)
Nicole Papen-Botterhuis
TNO Encapsulation Team
Advantages:
+ cheap, flexible process
+ continuous process
+ high throughput
+ small particles possible
(Possible) Disadvantages:
− incomplete encapsulation
− mix of particle sizes
New TNO technology: printing-drying
Alternative to spray drying
Droplet generation by inkjet technology
Nicole Papen-Botterhuis
TNO Encapsulation Team
monodisperse
drops
monodisperse
powders
drying
printing
viscosity upto 500 mPa·s
low shear
droplet size ~50 to 120 m
droplet size variation <1%
100 L/h using multiple nozzle head
Advantages:
+ Energy saving
+ Continuous process
+ Monodisperse powders, no fines
+ High density powders
(Possible) Disadvantages:
− incomplete encapsulation
Titel van de presentatie 14-11-2014 10:52
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Methods for droplet extrusion
Dropping
Vibration / coaxial air flow (Nisco)
Vibration / electrostatic (Büchi)
Jet cutter (Genialab)
Rotating extruder (SWRI, Sprai, PCT)
Multiple nozzles (Inotech, Brace, TNO)
Nicole Papen-Botterhuis
TNO Encapsulation Team
From R. Neufeld, Queen’s University
Lists are not exhaustive!
Encapsulation by fluidized bed coating
+ Suitable for a wide range of shell materials
+ Tuneable shell thickness
- Only for solid core materials
- Standard not suitable for particles < 50 µm
- Moderate pay-loads, especially for small particles
- Polydisperse products, agglomeration during coating
Typical (food) ingredients: vitamins, minerals, leavening agents
Also used for much larger food components (flakes, grains)
Also used for pharmaceutical & cosmetic applications
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Encapsulation by (complex) coacervation
+ High payloads possible
+ Good core-shell morphology
- Expensive & complex (batch) process
- Limited choice in shell materials
- Polydisperse capsules
Typical ingredients: flavour oils, also fish oil, vitamins etc.
Typical application areas of flavour microcapsules:
chewing gum, toothpaste, baked foods
Release mechanisms: sustained, mechanical or heat trigger
Nicole Papen-Botterhuis
TNO Encapsulation Team
Phase separation of one or more hydrocolloids by changing pH,
salt concentration, etc.
Core-shell particles by co-extrusion
Nicole Papen-Botterhuis
TNO Encapsulation Team
shell liquid
core liquid
piezoelectric
vibrating unit
Concentric nozzle to process core & shell material
Collection in non-solvent or coacervation bath
(Possible) Disadvantages:
− no dry powders
− large size (w.o. non-solvent)
− interaction between core & shell
material may occur at the nozzle
Advantages:
+ narrow size distribution
+ high payloads possible
+ good core-shell morphology
Non-solvent stream (optional)
Titel van de presentatie 14-11-2014 10:52
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Core-shell particles by encapsulation printing
New processing technology for microencapsulation:
Generate core droplet by inkjet technology
Encapsulation by a liquid film / curtain of shell material
Nicole Papen-Botterhuis
TNO Encapsulation Team
Example: Encapsulation of oil droplets
mechanical
release
shell = 5 – 8 m
Core: 82 – 86 %
oil droplets
aqueous solution of carrageenan and/or gelatin
Nicole Papen-Botterhuis
TNO Encapsulation Team
gelation
by cooling
Titel van de presentatie 14-11-2014 10:52
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Example: Encapsulation of water-soluble core
aqueous core droplets
(with model dye)
solid microcapsules
with waxy shell
molten
shell material
Nicole Papen-Botterhuis
TNO Encapsulation Team
solidification
by cooling
capsule diameter 70 µm
capsule diameter 400 µm
Size depends on parameters: flow rate, frequency, nozzle diameter
Tuning shell thickness / core-shell ratio
Shell thickness depends on flow rate of liquid film:
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Advantages & challenges encapsulation printer
+ High payloads
+ Continuous process
+ Suitable for wide range of materials (aqueous, oils/waxes, polymers,
solutions, dispersions)
+ High viscosities & temperatures possible
+ Mild process conditions (low T, shear) possible
+ Separate conditions for core & shell materials
+ Well-defined, homogeneous product properties
- No recycling of shell material yet
- Early stage development
Nicole Papen-Botterhuis
TNO Encapsulation Team
fluidized bed
Characteristics of encapsulation processes
Nicole Papen-Botterhuis
TNO Encapsulation Team
1 µm 10 µm 100 µm 1 mm
10%
50%
70%
90%
spray drying
melt
extrusion
complex
coacervation
simple
coacervation concentric
nozzle
Information adapted from: Zuidam et al, Encapsulation Technologies for Active Food Ingredients and Food Processing, 2010
encapsulation
printer
particle diameter
load (%)
30%
matrix type
core-shell
clay Intercalation
spray chilling
… or print-drying
sandwich type
Titel van de presentatie 14-11-2014 10:52
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Application Markets
Pharmaceuticals / Medical/ Animal Healthcare
Food / Nutraceuticals
Feed
Personal Care / Cosmetics
Home Care
Consumer Products
Agriculture / Aquaculture
Building materials / Paints & Coatings
Oil & Gas
Textiles
Energy storage
Nicole Papen-Botterhuis
TNO Encapsulation Team
Skip examples
Pharmaceuticals / Medical / Animal Healthcare
Sustained release (less pills, therapeutic window, from pills to implants)
Targeted release
Taste masking
Enteric release (protection against stomach)
Improved bioavailability
Animal/human cells (islets of Langerhans)
Nicole Papen-Botterhuis
TNO Encapsulation Team
LCTglobal.com
Titel van de presentatie 14-11-2014 10:52
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Encapsulation for Food Innovations
Flavors & Fragrances (aroma)
Immobilization during processing
Edible oils (omega-fatty acids)
Microorganisms (probiotics)
Levening agents
Vitamins
Shelf-life
Taste masking
Enteric release
Bioavailability
Quick dissolving powder
Free-flowing sugar
In situ generation of bactericides
Nicole Papen-Botterhuis
TNO Encapsulation Team
Personal Care/Cosmetics
Controlled release of fragrances: perfume, deodorant
Stabilization / Shelf-life
Bioavailability
Control of odour
Liquid to solid conversion
Cosmeto-textiles
Appearance
Marketing
Nicole Papen-Botterhuis
TNO Encapsulation Team
Pelletech Robert Blondel
Titel van de presentatie 14-11-2014 10:52
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Home care / Consumer goods
Detergents (enzymes)
Adhesives
Controlled release fragrance
Masking odour
Shelf-life
Self-healing
Scratch ‘n sniff
Visual indicators
Liquid crystal displays
Liquid to solid conversion
Nicole Papen-Botterhuis
TNO Encapsulation Team
Agriculture/Aquaculture
Herbicides/pesticides
Handling & Safety
Fertilizers
Pheromones
Plant growth promoting bacteria
Food supplementation
Structuring fish food
Bioavailability
Ingredient stabilization
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Chemical Industry
Lubricants
Adhesives (pressure-sensitive glue)
Enzymes
Inks/pigments
Flavors/Fragrances
Thermochromic dyes
Fermentative production of ethanol, biogas, lactic acid (microorganisms)
Aid in processing: Immobilization, easy to separate
Chemicals for Enhanced Oil Recovery
Phase Change Materials (PCMs) for textiles and energy storage
Nicole Papen-Botterhuis
TNO Encapsulation Team
Building Materials / Paints & Coatings
Controlled release biocide coatings
Pigments
Self-healing coatings
Phase change materials
Antimicrobial coatings
Thermochemical storage
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Nanoencapsulation
Why?
Optical clarity (drinks, motor oil)
Better surface interactions
Stability of suspensions
Higher penetration depth/uptake (cosmoceuticals, cell therapy)
How? Liposomes, micelles, molecular entrapment, nanoclay
Challenges:
Loading efficiency is a challenge for core-shell particles
Very thin shells needed: ALD, CVD techniques?
Fragility of capsules
Use of large amounts of surfactants for nanoemulsions
Nanopowders not easy to handle (nanotox, flowability)
Nicole Papen-Botterhuis
TNO Encapsulation Team
Conclusions
Encapsulation can provide a solution to enhance products
There are many encapsulation technologies and materials
Encapsulation process should be designed to meet exactly the product
requirements: ask a specialist if you are new in the field
Encapsulation is used in many application areas
Challenges
Better barrier materials/layers
Smaller particles with high loading
Milder encapsulation processes
Biobased encapsulation materials
Overcome regulations
Low-cost solutions
Nicole Papen-Botterhuis
TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Smart release of biocides in finishing materials for the sector of construction
The EU project “Axioma”
‘To develop, adapt and apply smart release concepts of eco-acceptable bio-inhibitors to extend service life of
finishing materials substantially.’
Moulds Algae
Axioma why?
14/11/2014 32
• Short bio-resistance of materials leads to early replacement
• Environmental legislation restricts use of biocides and chemicals (Biocidal product directive 98/08/EC) (Biocidal Product Regulation EU 528/2012, 1st Sept 2013)
Nicole Papen-Botterhuis TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Modified inorganic particles
1. swelling in a solvent (water)
2. cation exchange (modifier)
3. filtration + drying (de-swelling)
Possibility to load cationic
compounds onto clays, or anionic
compounds onto layered double
hydroxides.
Charge interactions can also take
place with neutral molecules (e.g.
amines).
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+
Nicole Papen-Botterhuis TNO Encapsulation Team
Change of equilibrium
Eversdijk, J., et al (2012). Development and evaluation of a biocide release system for prolonged antifungal activity in finishing materials. Progress in Organic Coatings, 74(4), 640-644.
Nicole Papen-Botterhuis TNO Encapsulation Team
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Titel van de presentatie 14-11-2014 10:52
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Sample preparation
Nicole Papen-Botterhuis TNO Encapsulation Team
Rain setup Loaded nanoclay
Coating
Biological and chemical tests
Improvement obtained by biological testing
Results paint
Nicole Papen-Botterhuis TNO Encapsulation Team
Titel van de presentatie 14-11-2014 10:52
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Results from gypsum
1. free biocide (red)
2. bound biocide with 100 wt% hydrophobic modifier (blue)
Nicole Papen-Botterhuis TNO Encapsulation Team
Fungal growth
5 times performance improvement
With Clay
Without Clay
Artificial rain tests and Fungal growth tests
Conclusion
Coating Technology and Encapsulation – Closely Connected!
Nicole Papen-Botterhuis
TNO Encapsulation Team
Encapsulation
Coatings capsules
coatings
can be applied to improve the functionality of
Titel van de presentatie 14-11-2014 10:52
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For more information please contact:
Nicole Papen-Botterhuis M.Sc., Ph.D.
TNO
Dept. Materials Solutions
PO Box 6235
5600 HE Eindhoven
The Netherlands
nicole.papen@tno.nl
+31 88 866 6234
Nicole Papen-Botterhuis
TNO Encapsulation Team
Groningen
Eindhoven
Den Helder
The Hague
Rijswijk
Delft
Apeldoorn
Leiden
Enschede
Hoofddorp
Utrecht
Soesterberg
Zeist
Helmond
• Independent Dutch nonprofit
research institute
• Approximately 3500 FTE
• TNO Encapsulation team
– 9 FTE core + 20 part-time
– New encapsulation processes
– New encapsulation materials
TNO connects people and knowledge to create
innovations that boost the sustainable competitive
strength of industry and well-being of society
TNO: Netherlands Organisation for Applied Scientific Research
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