Iasi Academic Days, Advances In Science Of Organic And Macromolecular Compounds, 29 september – 1 octomber, 2011, Iasi -Romania

Elena Părpăriţă, Raluca Nicoleta DARIE, Cornelia VASILE

“Petru Poni” Institute of Macromolecular Chemistry, 41A Grigore Ghiga Voda Alley, 700487, Iasi, Romania
elena.parparita@icmpp.ro

In the last twenty years, the use of lignocellulosic fibers as filler in the plastic industry has increased progressively. Thermoplastics are combined with lignocellulosic (wood) fillers to produce
wood/plastic composites. They provide several advantages such as low density, low cost, nonabrasive nature, possibility of high filling levels, low energy consumption, specific properties,
biodegradability, availability of a wide variety of fibers, and generation of a rural/agricultural-based economy. In addition, the utilization of recycled plastic and waste wood in the manufacturing of
such composites may help the environment protection by reducing the land filling and/or promoting the recycling.
In this study, composite based polypropylene (PP) and various vegetable residues such as grape seeds, eucalyptus wood, pine cones, grass energy, pulp brown stock (BSP), norway
spruce TMP, Brassica rape were obtained by melt processing. The obtained systems were mechanically tested, proving the efficiency of biomass use as reinforcements, the new
materials obtained, being more rigid.

 Isotactic polypropylene (PP) J 1100, ICEFS SA Savinesti: Tm = 170ºC; decomposition temperature

range: 205-430ºC, MFI = 2.4-3.2 g/10 min; isotactic index ~ 95%.
 Biomass (grape seeds, Eucalyptus wood (Euca), Pine Cones (PineC), Energy grass (Grass), pulp brown
stock (BSP), norway spruce (TMP), Brassica rape.
The eucalyptus wood, pine cones, grass and Brassica rape was dried at 80°C for 24 hours and grinded in • Stress-strain measurements were performed at room
a Retsch PM 200 planetary ball mill to become powder. An sieve was used to obtain an average filler size temperature on dumbbell-shaped samples (1 mm
of 0.16 mm. thickness), on an Instron Single Column Systems tensile
A solvent extraction method utilizing ether, water and ethylic alcohol, as solvent was used for the testing machine (model 3345) equipped with a 5kN load
extraction of fatty acids, tannins and flavonoids from grape seeds. For comparison three types of grape cell and activated grips, which prevented slippage of the
seeds were used : GS I, from which was extracted only fatty acids and tannins; GS II, from which was sample before break, operated according to SR EN ISO
extracted fatty acids, tannins and flavonoids and GSu, unextracted grape seeds. 527:1996. The used cross-head speed was 10 mm/min,
gauge length 40.0 mm;
• Impact tests have been performed according to SR EN
• The composites containing PP and vegetable residues were obtained by melt blending in the chamber ISO 179/2001, on a CEAST Impactor, equipped with a
of a Brabender mixer, at 175 °C. The systems were processed for 10 min at 60 rpm and their Charpy type hammer having 15 J energy.
corresponding torque-time curves have been recorded during processing. After the processing step, • Hardness tests have been performed using the
each sample was pre-melted for 5 min and then sandwiched in a Carver Press 4394, for 4 min, between Vickers method, with a 2.942 N load, for 12 sec.
two Teflon papers, and pressed at 130oC under a pressure of 200 bars, to obtain plates with thickness
of 1 mm for tensile tests and of 4 mm for impact bars, respectively. The specimens for mechanical tests
have been cut from the obtained plates.

Table 1. Processing characteristics and notations for studied samples Table 2. Tensile parameters for studied blends
Sample Young Modulus Strength at break Elongation at break
Sample TQmax (Nm) TQ1min (Nm) TQ5min (Nm) TQfin (Nm)
(MPa) (MPa) (mm)
PP 26.9 10 9.2 8.6
PP 1248 31 5
PP/Gsu 29.6 9.4 9.4 8
PP/Gsu 746 15 2
PP/GS I 59.6 8.2 6 5.8
PP/GS I 1075 20 2
PP/GS II 57.4 8.8 6.5 6.2
PP/GS II 1078 19 1
PP/Euca 58.3 8.5 6.1 6.1
PP/PineC 50.8 9 6.6 6.7 PP/Euca 1239 23 1

PP/Grass 46.4 8.5 7 6.8 PP/PineC 1180 19 1

PP/BSP 53.7 9.1 7.1 6.9 PP/Grass 1524 21 1
PP/TMP 25 7.2 3.9 3.9 PP/BSP 1437 25 2
PP/Brassica rape 64.2 17.1 11.7 10.7 PP/TMP 1232 19 1
TQmax – maximum torque; TQ1min – torque after 1 minute of mixing; TQ5min – torque after 5 minutes of mixing; TQfin – PP/Brassica rape 1315 20 1
torque at the end of processing
Comparred to pure PP, the Young Modulus of composites decreased for systems
The torque values decreased with increasing processing time because the mixing containing Gsu due to the grape seeds oil contained, but an increase of YM was
becomes easier by sample heating, and in the end achieved a stable value indicating the recorded when using Grass, BSP and Brassica rape as fillers. The effect of
complete blending of the components. Brassica rape fibers present in PP matrix biomass use as fillers is even more pronounced for elongation at break, which
constrain the rotors movement increasing the viscosity of the melted material related to decreases after introducing biomass in PP matrix, because of reinforcement effect
matrix. produced by filler material.

Table 3. Impact testing results for studied blends

Sample Impact strength (kJ/m2) Impact energy (J)
PP 17 0.6
PP/Gsu 7.2 0.2
PP/GS I 5.7 0.2
PP/GS II 6.4 0.2
PP/Euca 5.8 0.2
PP/PineC 6 0.2
PP/Grass 7.4 0.3
PP/BSP 10.1 0.4
PP/TMP 7.2 0.3
PP/Brassica rape 6.6 0.2

The composites containing biomass recorded a decrease in impact strength, as shown

in Table 3. The sample thickness was almost the same for all samples, therefore, the Hardness variation depending on the filling agent
energy required to fracture a sample had the same variation with that of the impact PP-biomass composites registered increased Vickers hardness values
strength. Due to the difference in polarity between matrix and fillers, compatibilizing related to PP matrix, proving the efficiency of biomass used as filling
agents would improve the impact results. agents, the new materials obtained being more rigid 
Polypropylene composites with vegetable residues have satisfactory mechanical properties Use of lower amount (<30%) and
compatibilizing agents will increase their performance. Type of vegetable residue has little influence than particle size.
 In the next studies thermal properties and pyrolysis behaviour will be studied.
Acknowledgements: This study is conducted with financial support from the EC Marie Curie Actions under the project People BIOFUEL- Reference: F. Mengeloglu , A Kabakcies, Determination of Thermal Properties and Morphology of Eucalyptus Wood Residue Filled
PIRSES-GA-2009-247550. Dr. Raluca N. Darie acknowledges the financial support of European Social Fund – „Cristofor I. Simionescu” Postdoctoral High Density Polyethylene Composites, Int. J. Mol. Sci., 9:107-119, 2008.
Fellowship Programme (ID POSDRU/89/1.5/S/55216), Sectoral Operational Programme Human Resources Development 2007 – 2013.