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2 08/04/2015
Biocomposite research at VTT
Competence
The well-equipped laboratory facilities and skilled
personnel enable top-level scientific research and
demanding contract research.
Strategy
International co-operation with customers and research
partners worldwide is the key to successful material
development.
Mission
VTT’s mission is to produce research and innovation
services that enhance the international competitiveness
of the partners in industry in Finland and abroad.
3 08/04/2015
COMPOSITES
- Biocomposites
- Nanocomposites and nanobiocomposites
- Structural composites (thermoset materials)
THERMOPLASTICS PROCESSING
- Foaming and extrusion technologies
- Nanodispersion for composites
- Non-destructive fibre dispersion
PERFORMANCE PLASTICS
- Flame retardancy
- Thermal and electrical conductivity
- Recyclability
- UV-protection
- Antimicrobial properties
- Barrier properties
- Wear resistance and low friction
Focus areas
3 08/04/2015
4 08/04/2015
Injection moulding
Thermo-Haake
MiniLab, Micro
Compounder
Tandem Extrusion Foaming Line
Berstorff
Compounding
Line
Plastics processing
Micro-scale melt processing
Small scale processing
Pilot scale processing
Pre- and Post-processing
Injection moulding
Extrusion (profile, cast and blow
film)
Extrusion and particle foaming
7 08/04/2015
Mechano-chemical fibre modification
VTT’s own method to modify fibres for composites
Allows addition of reactive additives safely on cellulose surface
Simultaneous additive mixing and fibre compacting for compounding
Low friction even with high dry material content (>70%)
Saves energy and solvent compared to normal solvent processing
methods
Can be used as pre-processing method to enhance enzymatic
modification
Suitable for wood cellulose, saw dust, wood chips, agro fibres etc.
Very high output even with small equipment (180 kg/h)
8 08/04/2015
Mechano-chemical fibre modification
Used for :
Fibre pulp processing and modification in dry material content up to 40%.
Easy cost and energy saving way to add plasticizers before compounding
Reactive plasticizer addition on fibre surface
Monomer addition for reactive compounding / polymerisation during compounding
Fibre surface modification (fibrillation) for different purposes, fibrillation degree can be adjusted
Pre-processing to enhance enzymatic modification
Pre-processing for cellulose degradation for sugars (improved yield)*
Can be combined with compounding or reactive compounding processes in composite manufacturing
* Patent application WO 2012/113990 A1
9 08/04/2015
Combined process for fibre modification
and plasticization of PLA
Mechano-chemical cellulose modification method developed at
VTT:
- Is easy, safe, costs, energy and solvent saving method
working with low friction suitable for natural materials
(cellulose, saw dust, agro fibres etc.) even with high dry material
content up to 75%.
- Introduction of additives, their mixing and improved attachments
on fibre
TWO RELATED PATENT APPLICATIONS: 1. Sivonen, E., Valta, K., Seulalevypuristin, Finnish patent application FI20106340 left December 17th 2010.
2. Immonen, K., Sivonen, E., Hulkko, J., Valta, K., Aalto, S., Pitkänen, P., Salorinne, K., Process for manufacturing a thermoformed
plasticized composite containing celulose fiber and a moldable polymer, WO 2012/117165 A2
Results
- Thermoformed sheet materials with PLA and 36% cellulose fibre
content were made
- Tensile strength was improved by 26%
- Impact strength was improved by 100%
Thermoformed sheets
Good connection between
polymer and fibre
Fibre fibrillation
Additional information: Kirsi Immonen
10 08/04/2015
Example of reactive plasticizers added on birch cellulose
0
5
10
15
20
25
30
35
Birch r
ef.
Lin
ear
OH
Epoxid
e1(B
ranched)
OH
2
Epoxid
e2(e
lasto
mer)
Epoxid
e3(d
i)
Dis
pers
ant1
Epoxid
e4
Anhydride1
Lacto
ne
Anhydride2
Epoxid
e5(S
i)
Dis
pers
ant2
VT
T a
nhydride
VT
T e
poxid
e1
VT
T e
poxid
e2
Imp
act
str
en
gth
, kJ/m
2
Impact strength results for PLA birch pulp composites with 7.5%
additive and a fibre content of 30%
* Related patent applications FI20115218 and FI20106340
11 08/04/2015
Chemo-enzymatic fibre modification
for biocomposites (EU-WoodWisdom-Net project FunFireBic - Functional Fibre Reinforced Biocomposites)
Enzyme activated functional chemical attachment on fibre surface
Chemo-enzymatically modified lignin containing fibre (e.g. mechanical
fibre) is applicable in the wood fibre-biopolymer biocomposites.
Injection moulded fibre-biopolymer compounds with 40% modified fibre
Better processability and improved fibre dispersion in polymer matrix
e.g. PLA-CTMP composites:
→ 50% increase in tensile strength
→ 130% increase in impact strength
Improved fibre
Dispersion in
PLA and PHB
This modification method is successfully applied also for flax-fibres in
combination with thermosetting epoxy-composites.
Additional information: Anna Suurnäkki or Kirsi Immonen
13 08/04/2015
Thermoplastic lignin composites FuBio Joint Research 2 (FuBio JR2) project
Lignin: Softwood kraft lignin from Valmet (LignoBoost)
Plasticizers: Biobased plasticiser and polyethylene glycol (PEG)
Fiber: Softwood TMP
14 08/04/2015
Lignin composites (Fubio JR2)
Lignin composites
Process chain
Cellulose
fibres
Lignin extraction by
Kraft process Plasticisation
Compounding
with fibres
Injection moulding &
extrusion
Lignin Plasticized
lignin
Ojala et al. Thermoplastic lignin and reinforcing cellulose fiber composites for
advanced biocomposite applications, Programme Report 2011-2014, Future
Biorefinery Joint Research 2, 2014.
Ojala et. al. Foam-laid thermoplastic composites based on kraft lignin and softwood
pulp, J. Renew. Mater, 2014, DOI: http://dx.doi.org/10.7569/JRM.2014.634126
15 08/04/2015
Injection moulded thermoplastic lignin composites
0
5
10
15
20
25
30
0 0,1 0,2 0,3 0,4 0,5 0,6
Ten
sile
str
engt
h /
MP
a
Lignin weight fraction
0
1
2
3
4
5
6
7
0 0,1 0,2 0,3 0,4 0,5 0,6
Mo
du
lus
/ G
Pa
Lignin weight fraction
0
2
4
6
8
10
12
0 0,1 0,2 0,3 0,4 0,5 0,6
Stra
in a
t b
reak
/ %
Lignin weight fraction
0
5
10
15
20
25
0 0,1 0,2 0,3 0,4 0,5 0,6Imp
act
stre
ngt
h /
kJ
/ m
2
Lignin weight fraction
• Composition: kraft lignin / biobased plasticiser / wood fibres
• 20 wt% wood fibre content in all samples
16 08/04/2015
Thermoplastic lignin composites Biobased plasticiser vs PEG
• 30 wt% TMP fiber content
• Optimized lignin / plasticizer ratios
27
29
5,2 5,9
0,6 0,5 1,7
4,2
Biobased PEG
Tensile Strength (MPa)
Young's modulus (GPa)
Strain at break (%)
Impact Strenght (kJ/m2)
17 08/04/2015
Water absorption of thermoplastic lignin composites Bio-based plasticiser vs PEG
• 20 wt% TMP reinforcement
• PEG dissolves from the composites
0
10
20
30
40
50
0,0 0,5 1,0 1,5 2,0 2,5
Wei
ght
chan
ge /
%
Time / weeks
Biobased
PEG
18 08/04/2015
Property PP + Wood1 Lignin + PEG + TMP Lignin + biobased
plasticiser+ TMP
Tensile strength (MPa) 37 29 30
Stiffness (GPa) 3.0 6.5 5.4
Impact strength (kJ/m2) 15 4.4 2.0
1Ichazo et al., Compos. Struct., 2001
Comparison:
40% Wood fibers + PP
vs
30% TMP + lignin + biobased plasticiser
vs
30% TMP + lignin + PEG
20 08/04/2015
Expanded and extrusion foamed bio-based thermoplastics
Sustainability by replacing oil-based components
Light-weight, high insulation
100% bio-based
Applications in packaging, construction, and transport
Process and development from laboratory to pilot scale
Light weight materials with bio-based foams
21 08/04/2015
Extrusion Foaming Possibilities at VTT
Thermoplastic foam development from small scale to pilot scale
- Batch foaming equipment: Overall foamability of polymers with various blowing agents (BA’s)
can be evaluated with less than 10 g of sample
- Laboratory scale single screw extrusion foaming line: Extrusion foaming conditions
(temperatures, BA content, etc.) in continuous process can be evaluated with ~2-5 kg of polymer
- Pilot scale tandem extrusion foaming line: Foamed sheet and board can be produced for
industrial testing purposes with ~50-100 kg of polymer
22 08/04/2015
Extrusion foamed biocomposites
and bio-based thermoplastics
OSIRYS project: Safe, energy-efficient and affordable new eco-innovative materials for
building envelopes and/or partitions to provide a healthier indoor environment
Within the project, VTT develops an interior
multilayer structure from light foam
biocomposite with light-weight, and excellent
mechanical, thermal insulation and sound
absorption and insulation properties
Porous wood fibre webs produced by
foam laid forming
Physically expanded, bio-based closed cell
foam produced by thermoplastic extrusion
process Cell structure of extrusion foamed
biocomposite sample produced in VTT
lab-scale extrusion foaming line