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Outline

Biopolymer based Nanocomposites;


Processing and Properties 1. Project goal

2. Materials and principles behind nanocomposite processing

3. Experience from extrusion so far


Daniel Bondeson & Kristiina Oksman
4. Optimization of the isolation of nano crystals from microcrystalline
cellulose by sulfuric acid hydrolysis

5. Progress plan and publications

Department of Engineering Design and Materials Department of Engineering Design and Materials

Outline Materials

Nanoreinforcement:
Produce biopolymer based nanocomposites - MCC (micro crystalline cellulose) [Asahi Kasei Corp.]
with industrially viable process methods
- Chitin [Sigma-Aldrich]

Matrix:

continous process - PLA (polylactic acid) [Cargill Dow]


(such as extrusion) - CAB (cellulose acetate butyrate) [Eastman]
- starch polymers [Novamont]

Gilde

Department of Engineering Design and Materials Department of Engineering Design and Materials

1
Challenges in making Nanocomposites Characterization methods

•Mechanical properties
Problems?
max dispersion in
less than 1-2 min •Rheology

•Structure (OM, SEM, TEM, AFM) Ingvild Kvien


1. Compatibility between Bjørn Steinar Tanem
nanoreinforcement and •X-ray
polymer

2. Adequate shear forces to


break agglomerates
appart

Department of Engineering Design and Materials Department of Engineering Design and Materials

Extrusion process Extrusion process

1. Materials: PLA (matrix) 2. Feeding MCC as dispersion and ”dry”


MCC (dry)
MCC (reinforcement) +
MCC
pellets (suspension)
pellets

compatibilizer (MA-PLA)

plasticizer (PEG)

1. PLA 8. PLA + MA-PLA + MCC/DMAc/LiCl


2.
3.
PLA + MA-PLA
PLA + PEG
9.
10.
PLA + PEG + MCC/DMAc/LiCl
PLA + MA-PLA + PEG + MCC/DMAc/LiCl
3. Used 2 different screw configuration
4. PLA + MA-PLA + PEG 11. PLA + DMAc/LiCl
5. PLA + MCC 12. PLA + H2O
6. PLA + MA-PLA + MCC 13. PLA + MA-PLA + MCC/H2O
7. PLA + MCC/DMAc/LiCl

Department of Engineering Design and Materials Department of Engineering Design and Materials

2
Extrusion process Cellulose whisker optimization

Conclusions: Sulfuric acid hydrolysis of MCC, optimization:


- Using of response surface methodology
• need isolation/separation of MCC
Factors:
• PLA-matrix degradation by DMAc/LiCl 1. sulfuric acid concentration Responses:
2. hydrolysis time • Yield
• suspension feeding probably involve • median particle
3. hydrolysis temperature
agglomeration of cellulose at feeding point size
4. MCC start concentration • sulfate groups
• need compatibility between PLA and cellulose 5. sonication time

• need correct screw configuration

Correlations used to set up a model

Department of Engineering Design and Materials Department of Engineering Design and Materials

Cellulose whisker optimization Progress plan and publications


Hydrolysis optimization of cellulose whiskers:
Tasks 2003 2004 2005 2006
Maximize: 1.Literature studies *** ****
2.Nanofiber separation *********** ******
yield 3.Nanocomposite processing ******* ************** ******
4.Analysis of enhanced structure and properties ******* ************** ******
start concentration of MCC 50 µm 5.Preparation of PhD-thesis and defence ********

OM (×100)
Minimize:
sulfuric acid concentration
hydrolysis time put in model Publications
500 nm
sonication time and optimize
AFM 2 µm
1. Optimization of the Isolation of Nano Crystals from Microcrystalline
Cellulose by Acid Hydrolysis (under preparation)

2. Optimization of the preparation of nano crystals from microcrystalline


suggestions of optimized cellulose in aqueous suspension Conference in San Diego,
treatment conditions March 2005
Birefrigence

Department of Engineering Design and Materials Department of Engineering Design and Materials