1. ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 1 Development and design of recycling-reuse of composite components PROJECT Eco-Houses Based on Eco-Friendly Polymer Composite Construction Materials - ECO-PCCM 11 OKTOMVRI EUROKOMPOZIT ISO 9001:2000

2. 2 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006AIMS Investigation of the recycling ability of the PP and PLA matrix Application of the recycled matrix for production of the Rice Straw - composites and Kenaf - composites Investigation of the recycling ability of the Rice Straw - composites and Kenaf - composites

3. 3 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 1 Preparation and characterization of PP matrix by recycling one and two times and PLA matrix by recycling once Part 2 Preparation and characterization of the composites based of PP recycled (one and two times) matrix and composites based on PLA recycled (one time) matrix Part 3 Preparation and characterization of the Rice Straw based composites by recycling one and two times Part 4 Preparation and characterization of the Kanaf based composites by recycling one and two times SUMMARY

4. 4 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 PART 1: Preparation and characterization of the recycled matrix Preparation PP matrix - extruded one and two times (PP x1 and PP x2) into strips with a single screw extruder at 200 o C - the obtained recycled matrices were cut in pellets form to perform the sheets - thay have been molded by thermo compression at T= 185 o C, t=10 min with continuous increasing pressure up to 10 000 pounds. PLA matrix - extruded one time (PLA x1) into strips with a single screw extruder at 190 o C - extruded one time (PLA x1) into strips with a single screw extruder at 190 o C - the obtained recycled matrix was cut in pellets form to perform the sheets - it has been molded by thermo compression at T= 175 o C, t=10 min with continuous increasing pressure up to 10 000 pounds. MARIA’S HANDS!

5. 5 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 PART 1: Preparation and characterization of the recycled matrix From the recycled matrices the plates with thickness 3 mm are produced The flexural tests are performed on unnotched (Young’s Modulus) and on notched samples (Kc and Gc) TGA analyses Characterization

6. 6 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 The flexural tests Stress at peak, MPa Standard Deviation Modulus, MPa Standard Deviation PP neat 51,55,51081120 PP x1 52,82,1130564 PP x2 49,52,91341101 PLA neat 32,03,82416204 PLA x1 32,06,12431193 K c, MN -3/2 m G c, kJ/mm 2 PLA neat 1,220,61 PLAx11,150,53

7. 7 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Recycling properties

8. 8 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: recycled PP TGA analyses: recycled PP T d [ o C] (weight residual) (weight residual) ~ 90 % T d [ o C] (weight residual) ~ 50 % T d [ o C] (weight residual) ~ 10 % PP neat 377,60 (90,38 %) 429,32 (50,38 %) 449,79 (10,38 %) PP x1 357,49 (90,89 %) 414,67 (50,87 %) 438,64 (10,89 %) PP x2 354,87 (86,37 %) 403,64 (46,37 %) 427,15 (11,37 %) PP neat PP x1 PP x2

9. 9 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGAanalyses: recycled PLA T d [ o C] (weight residual) ~ 90 % T d [ o C] (weight residual) ~ 50 % T d [ o C] (weight residual) ~ 10 % PLA neat 332,22 (90,53 %) 362,52 (50,53 %) 380,07 (10,53 %) PLA x1 329,68 (90,54 %) 364,21 (50,54 %) 382,98 (10,54 %) PLA x1 PLA neat

10. 10 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 CONCLUSION for the first part From the investigation of the recycled ability of the PP matrix and PLA matrix can conclude: recycled matrices can be use for production of the composites

11. 11 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 2: Preparation and characterization of the composites based on PP recycled and composites based on PLA recycled PP recycled based composites wt / wt PP/RS/CA 60/30/10 wt / wt wt / wt PPx1/RS/CA 60/30/10 wt / wt wt / wt PPx2/RS/CA 60/30/10 wt / wt wt / wt PP/kenaf/CA 60/30/10 wt / wt wt / wt PPx1/kenaf/CA 60/30/10 wt / wt -The obtained recycled PP matrices were mixed in a Brabender together with the copuling agent (PP-g-MA) and with Rice Straw and Kenaf fibers (reactive blending) -melt mixing in Brabender at 180 o C, time 10 min: PP; dry rice straw; PP; dry rice straw; PPx1; } + CA (3 min) + { dry kenaf fibers; (7 min) PPx1; } + CA (3 min) + { dry kenaf fibers; (7 min)PPx2; - the obtained composites were cut in pellets form to perform the sheets - thay have been molded by thermo compression at T= 185 o C, t=10 min with increasing pressure up to 10 000 pounds. Preparation

12. 12 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 2: Preparation and characterization of the composites based on PP recycled and composites based on PLA recycled PLA recycled based composites wt / wt PLA / RH / CA 65/30/5 wt / wt wt / wt PLA x1 / RH / CA 65/30/5 wt / wt -melt mixing in Brabender at 170 o C, time 10 min: PP; dry rice straw; PP; dry rice straw; PLAx1; } + CA (3 min) + { dry kenaf fibers; (7 min) PLAx1; } + CA (3 min) + { dry kenaf fibers; (7 min) - the obtained composites were cut in pellet form to perform the sheets - thay have molded by thermo compression at T= 185 o C, t=10 min with continuous adding a pressure up to 10 000 pounds. Preparation

13. 13 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 From the obteined composites the plates with thickness 3 mm have done The flexural tests are performed on unnotched (Young’s Modulus) and on notched samples (Kc and Gc) TGA analyses SEM analyses on the cryogenically fractured surface Characterization Part 2: Preparation and characterization of the composites based on PP recycled and composites based on PLA recycled

14. 14 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 The flexural tests for PP recycled based composites Stress at peak, MPa Standard Deviation Modulus, MPa Standard Deviation PP / RS / CA 60/30/10 wt / wt 42,63,4194182 PPx1 / RS / CA 60/30/10 wt / wt 42,21,2182541 PPx2 / RS / CA 60/30/10 wt / wt 39,64,6184263 PP / Kenaf / CA 60/30/10 wt / wt 51,34,8210668 PPx1 / Kenaf / CA 60/30/10 wt / wt 51,13,02346204

15. 15 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 The flexural tests for PLA recycled based composites Stress at peak, MPa Standard Deviation Modulus, MPa Standard Deviation PLA / RS / CA 65/30/5 wt / wt 28,86,63031182 PLAx1 / RS / CA 65/30/5 wt / wt 14,81,32275457 K c, MN -3/2 m G c, kJ/mm 2 PLA/RH/CA 65 / 30 / 5 1,050.42 PLAx1/RH/CA 0.570.17

16. 16 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Recycling properties

17. 17 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Recycling properties PLA/RS/CA PLAx1/RS/CA The color is darker than the composite with neat PLA

18. 18 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: PP recycled based composites TGA analyses: PP recycled based composites T d [ o C] (weight residual) ~ 90 % T d [ o C] (weight residual) ~ 50 % T d [ o C] (weight residual) ~ 10 % PP / RS / CA 344,43 (89,74 %) 411,21 (49,74 %) 452,17 (9,74 %) PP x1/RS/CA 309,09 (87,51 %) 385,22 (47,51 %) 458,82 (12,51 %) PP x2/RS/CA 343,53 (86,82 %) 405,97 (46,82 %) 475,27 (11,82 %) PP x2/RS/CA PP x1/RS/CA PP /RS/CA

19. 19 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: PP and PLA recycled based composites TGA analyses: PP and PLA recycled based composites T d [ o C] (weight residual) ~ 90% T d [ o C] (weight residual) ~ 50 % ~ 50 % T d [ o C] (weight residual) ~ 10 % PP / Kenaf / CA 356,81 (85,94 %) 408,94 (50,94 %) 441,96 (10,94 %) PP x1/ Kenaf / CA 356,92 (86,98 %) 412,35 (51,98 %) 443,77 (11,98 %) PLA x1/ RH / CA 299,42 (88,41 %) 341,70 (48,41 %) 529,70 (13,41 %) PLAx1 /RS/CA PP /Kenaf/CA PPx1 /Kenaf/CA

20. 20 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses A B C A ) PP/RS/CA B ) PPX1/RS/CA C ) PPX2/RS/CA

21. 21 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses AB A ) PP/Kenaf/CA B ) PPX1/Kenaf/CA

22. 22 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses A A ) PLAX1/RS/CA

23. 23 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 3: Preparation and characterization of the Rice Straw based composites by recycling one and two times RS based composites wt / wt PP/RS/CA (X1) 60/30/10 wt / wt wt / wt PP/RS/CA (X2) 60/30/10 wt / wt wt / wt PLA/RS/CA (X1) 60/30/10 wt / wt wt / wt PLA/RS/CA (X2) 60/30/10 wt / wt -melt mixing in Brabender at 180 o C for PP and 170 o C for PLA, time 10 min: PP + CA (3 min) + dry rice straw; (7 min) PP + CA (3 min) + dry rice straw; (7 min) PLA + CA (3 min) + dry rice straw; (7 min) - the RS composites have been recycled one and two times - the obtained composites were cut in pellets form to perform the sheets - thay have been molded by thermo compression at T= 185 o C (T= 175 o C), t=10 min with increasing pressure up to 10 000 pounds. Preparation

24. 24 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 3: Preparation and characterization of the Rice Straw based composites by recycling one and two times Characterization From the obtained composites the plates with thickness 3 mm have done The flexural tests performed on unnotched (Young’s Modulus) and on notched samples (Kc and Gc) TGA analyses SEM analyses on the cryogenically fractured surface

25. 25 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 The flexural tests for recycled RS based composites Stress at peak, MPa SD Modulus, MPa SD K c, MN -3/2 m G c, kJ/mm 2 PP / RS / CA 60/30/10 wt / wt 42,63,4194182 PP / RS / CA (x1) 60/30/10 wt / wt 44,83,01884163 PP / RS / CA (x2) 60/30/10 wt / wt 38,57,2191059 PLA / RS / CA 65/30/5 wt / wt 26,86,630311821,050,42 PLA / RS / CA (x1) 65/30/5 wt / wt 12,14,832113810,530,12 PLA / RS / CA (x2) 65/30/5 wt / wt 10,72,533071760,450,11

26. 26 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Recycling properties

27. 27 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: Recycled RS composites TGA analyses: Recycled RS composites T d [ o C] (weight residual) ~ 90 % T d [ o C] (weight residual) ~ 50 % T d [ o C] (weight residual) ~ 10 % PP / RS / CA 344,43 (89,74 %) 411,21 (49,74 %) 452,17 (9,74 %) PP / RS / CA (x1) 336,66 (90,91 %) 409,93 (50,91 %) 471,04 (10,91 %) PP / RS / CA (x2) 322,63 (86,99 %) 389,01 (46,99 %) 455,28 (11,99 %) PP /RS/CA PP/RS/CA (x2) PP/RS/CA (x1)

28. 28 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: Recycled RS composites TGA analyses: Recycled RS composites T d [ o C] (weight residual) ~ 90 % T d [ o C] (weight residual) ~ 50 % T d [ o C] (weight residual) ~ 10 % PLA neat 332,22 (90,53 %) 362,52 (50,53 %) 380,07 (10,53 %) PLA / RS / CA (x1) 294,40 (86,50%) 328,52 (46,50 %) 517,28 (11,50%) PLA / RS / CA (x2) 289,08 (88,08%) 328,47 (48,08 %) 531,14 (13,08 %) PLA/RS/CA (x1) PLA/RS/CA (x2)

29. 29 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses A B C A ) PP/RS/CA B ) PP/RS/CA (x1) C ) PP/RS/CA (x2)

30. 30 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses A A ) PLA/RS/CA (x1) B ) PLA/RS/CA (x2) B

31. 31 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Part 3: Preparation and characterization of the Kenaf based composites by recycling one and two times RS based composites wt / wt PP/Kenaf/CA (X1) 60/30/10 wt / wt wt / wt PP/Kenaf/CA (X2) 60/30/10 wt / wt -melt mixing in Brabender at 180 o C, time 10 min: PP + CA (3 min) + dry kenaf; (7 min) - the RS composites have been recycled one and two times - the obtained composites were cut in pellets form to perform the sheets - thay have been molded by thermo compression at T= 185 o C, t=10 min with increasing pressure up to 10 000 pounds. Preparation

32. 32 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 The flexural tests for recycled Kenaf based composites Stress at peak, MPa StandardDeviat ion Modulus, MPa Standard Deviation PP / Kenaf / CA 60/30/10 wt / wt 51,34,8210668 PP / Kenaf / CA (x1) 60/30/10 wt / wt 51,89,12531179 PP / Kenaf / CA (x2) 60/30/10 wt / wt 48,74,7257580 Recycling properties

33. 33 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses: Recycled Kenaf composites TGA analyses: Recycled Kenaf composites T d [ o C] ~ 90 % T d [ o C] ~ 50 % T d [ o C] ~ 10 % PP / Kenaf / CA 340,57 (90,94 %) 408,94 (50,94 %) 441,96 (10,94 %) PP/Kenaf/CA (x1) 343,10 (91,11 %) 413,71 (51,11 %) 447,01 (11,11 %) PP/Kenaf/CA (x2) 344,28 (91,02 %) 414,94 (51,02 %) 448,84 (11,02 %) PP /Kenaf/CA PP/Kenaf/CA (x1) PP/Kenaf/CA (x2)

34. 34 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 TGA analyses T d [ o C] ~ 50 % w.r. PLA neat 362,52 PLA x1 364,21 PLA (x1) / RS / CA 337,61 PLA / RS / CA (x1) 328,52 PLA / RS / CA (x2) 328,47 PP neat 429,32 PP/RS/CA (x1) 409,93 PP/RS/CA (x2) 389,01 PP/Kenaf/CA (x1) 413,71 PP/Kenaf/CA (x2) 414,94 } The termal stability is the same for the neat PLA and recycled PLA } The termal stability is the same for PLA/RS composites recycled one and two times } } The termal stability for PLA/RS composites is lower than PP/RS composites

35. 35 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses A B C A ) PP/Kenaf/CA B ) PP/Kenaf/CA (x1) C ) PP/Kenaf/CA (x2)

36. 36 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 CONCLUSION PP recycled and PLA recycled based composites were produced by reactive blending, The flexural properties of the PP recycled based composites are very close to flexural properties of the composite with neat PP, The flexural properties of the PLA recycled based composite are lower (about 50%) compared to composite with neat PLA, The flexural properties of the PLA recycled based composite are lower (about 50%) compared to composite with neat PLA, The termal stability of the PP recycled and PLA recycled composites is slightly lower compared to composite with neat matrix, Recycled PP matrix can be use for production of the composites Recycled PP matrix can be use for production of the composites

37. 37 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 Recycled RS and Kenaf based composites were produced by reactive blending, Recycled PP/Kenaf composites show higher flexural properties compared to PP/RS composites, Recycled PLA/RS composites show lower flexural properties compared to PP/RS and PP/Kenaf composites, The termal stability of the recycled PP/Kenaf and PP/RS composites is slightly lower compared to base composite without recycling, The termal stability of the recycled PLA/RS composites is lower compared to base composite without recycling CONCLUSION

38. 38 ECO-PCCM Fifth Meeting, Barcelona, Spain, September 4-5, 2006 SEM analyses show that in all composites the interaction between matrix and RS or Kenaf are very good, resulting in high interfacial adhesion. Recycled PP matrix can be use for production of the composites Recycled PP/RS and PP/Kenaf composites are ability for reuse as composite components CONCLUSION