Preparation and characterization of pla pbat organoclay composites
1. PREPARATION AND
CHARACTERIZATION OF
POLY(LACTIC ACID)/POLY(BUTYLENE
ADIPATE-CO-THEREPTHTHALATE)
NANOCOMPOSITES
by
Mohd Junaedy Osman (GS21850)
Dr Nor Azowa Ibrahim
Prof Dato’ Dr Wan Md Zin Wan Yunus
Dr Jamaliah Sharif (Nuclear Agency Malaysia)
2. Introduction.
• Environmental problem has been arising ever since the usage
of plastic was introduced. For this reason, there is an urgent
need to study and to develop renewable source-based
biopolymers (able to degrade via a natural composting
process).
• One of the ways to diminish the effect of these problems was
to use biodegradable polymer or also called Green Polymer.
3. Poly(lactic acid) (PLA)
• PLA is a biodegradable, thermoplastic, aliphatic polyester derived
from renewable resources, (corn starch or sugarcanes).
• Standard grade PLA has high modulus and strength comparable to
that many petroleum based plastics (brittle).
PLA monomer
4. Poly(butylene adipate-co-therephtlate) (PBAT)
• PBAT (Ecoflex ) is an aliphatic-aromatic copolyester, which is fully
biodegradable. (Jiang et al. 2006).
• It is a flexible plastic designed for film extrusion and extrusion
coating.
PBAT monomer.
5. Objectives.
• To prepare organoclay through ion exchange technique
process with various type of alkyl ammonium ion.
• To characterize the organoclay produced.
• To study the effect of adding PBAT on the mechanical
and thermal properties of PLA/PBAT nanocomposites.
• To investigate the effect of organoclay on mechanical,
thermal and morphology of PLA/PBAT nanocomposites.
6. •The production of polymer materials has grown rapidly in the past 50 years. The
versatility of plastics is not exceeded by any other class of materials, guarantees that
polymers will continue to be very important in the future.
•The problem was the creation of phase separated mixture or immiscible blends. The
immiscible blends can be easily classified by looking through its morphology and
dynamics mechanical analysis.
Literature Review
7. Method and Result
•Preparation of organoclay
•Preparation of PLA/PBAT blends
•Preparation of PLA/PBAT nanocomposites
•Effect of type of clay
•Effect of clay loading
9. Preparation of organoclay
• 2 types of organoclay prepared.
–ODA-MMT
–DDOA-MMT
• The organoclay were prepared according to the
published method with slight modification (Tabtiang
et al., 2000; Pospisil et al., 2004; Capkova et al.,
2006)
45. 0.00E+00
1.00E+08
2.00E+08
3.00E+08
4.00E+08
5.00E+08
6.00E+08
7.00E+08
-50 -30 -10 10 30 50 70 90
Temperature (
o
C)
LossModulusG"(Pa)
PLA/PBAT
PLA/PBAT/Na-MMT
PLA/PBAT/ODA-MMT
PLA/PBAT/DDOA-MMT
PLA/PBAT/C 20A
0.00E+00
2.00E+07
4.00E+07
6.00E+07
8.00E+07
1.00E+08
1.20E+08
1.40E+08
1.60E+08
1.80E+08
2.00E+08
-30 -25 -20 -15 -10 -5 0 5 10
Temperature (
o
C)
LossModulusG"(Pa)
PLA/PBAT
PLA/PBAT/Na-MMT
PLA/PBAT/ODA-MMT
PLA/PBAT/DDOA-MMT
PLA/PBAT/C 20A
The effect of type of clay on loss modulus
46. Tg for different type of clay
Sample Identification Tg PLA (o
C) Tg PBAT (o
C)
PLA/PBAT 68.1 -23.0
PLA/PBAT/Na-MMT 64.3 -10.1
PLA/PBAT/ODA-MMT 62.3 -15.5
PLA/PBAT/DDOA-MMT 61.7 -12.2
PLA/PBAT/C 20A 63.4 -12.5
47. 0
20
40
60
80
100
200 250 300 350 400 450 500 550
Temperature (o
C)
Weight%(%)
(a)
(b)
(c)
(d)
(e)
TGA curve for (a) PLA/PBAT, (b) PLA/PBAT/Na-MMT, (c) PLA/PBAT/C 20A
(d) PLA/PBAT/DDOA-MMT and (e) PLA/PBAT/ODA-MMT
48. -22
-17
-12
-7
-2
200 250 300 350 400 450 500 550
Temperature (o
C)
DerivativesWeight%(%/m)
(a)
(b)
(c)
(d)
(e)
DTG curve for (a) PLA/PBAT, (b) PLA/PBAT/Na-MMT, (c) PLA/PBAT/C 20A,
(d) PLA/PBAT/DDOA-MMT and (e) PLA/PBAT/ODA-MMT
49. The thermal degradation for PLA/PBAT and PLA/PBAT/nanocomposites
with various type of clay
Sample
Tonset
(o
C) T50
(ºC) Tmax
(ºC)
PLA/PBAT 275.39 318.78 321.52
PLA/PBAT/Na-MMT 286.71 325.27 329.38
PLA/PBAT/ C 20A 300.36 332.13 334.93
PLA/PBAT/DDOA-MMT 307.52 334.19 335.37
PLA/PBAT/ ODA-MMT 310.36 336.09 336.98
50. (a) (b)
(c) (d)
SEM images of (a) PLA/PBAT/ODA-MMT, (b) PLA/PBAT/DDOA-MMT,
(c) PLA/PBAT/C 20A and (d) PLA/PBAT/Na-MMT
51. (a) (b)
(c) (d)
200 nm200 nm
200 nm 200 nm
TEM images for (a) PLA/PBAT/Na-MMT, (b) PLA/PBAT/ODA-MMT,
(c) PLA/PBAT/DDOA-MMT and (d) PLA/PBAT/C 20A (Magnification 10000x)
52. 0
0.5
1
1.5
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
Time (days)
Waterabsorption
percentage(%)
PLA/PBAT PLA/PBAT/Na-MMT PLA/PBAT/ODA-MMT
PLA/PBAT/DDOA-MMT PLA/PBAT/C20A
Water absorption percentage of PLA/PBAT incorporation with different type of clay
53. Percentage water uptake PLA/PBAT incorporation with different type of clay
Time (days)
Sample 0 2 4 8 16
PLA/PBAT 0 1.22 1.45 1.45 1.45
PLA/PBAT/Na-MMT 0 1.32 1.51 1.52 1.52
PLA/PBAT/ODA-MMT 0 1.20 1.44 1.44 1.44
PLA/PBAT/DDOA-MMT 0 1.21 1.45 1.45 1.45
PLA/PBAT/C 20A 0 1.21 1.44 1.44 1.44
54. 0
2
4
6
8
10
12
14
16
0 2 4 6 8 10 12
Time (weeks)
Weightlosspencentage(%)
PLA/PBAT PLA/PBAT/Na-MMT
PLA/PBAT/ODA-MMT PLA/PBAT/DDOA-MMT
PLA/PBAT/C 20A
Weight loss percentage of PLA/PBAT incorporation with different type of clay
55. Percentage weight loss PLA/PBAT incorporation with different type of clay
Time (weeks)
Samples 0 3 6 9 12
PLA/PBAT 0.00 2.33 2.52 2.69 2.76
PLA/PBAT/Na-MMT 0.00 2.39 2.62 2.75 2.82
PLA/PBAT/ODA-MMT 0.00 2.23 3.77 5.63 8.41
PLA/PBAT/DDOA-MMT 0.00 2.03 3.56 5.25 7.96
PLA/PBAT/C 20A 0.00 2.00 3.56 4.81 7.62
65. 0.00E+00
1.00E+08
2.00E+08
3.00E+08
4.00E+08
5.00E+08
6.00E+08
-50 -30 -10 10 30 50 70 90
Temperature (
o
C)
LossModulusG"(Pa)
PLA/PBAT
PLA/PBAT/0.1 ODA-MMT
PLA/PBAT/0.3 ODA-MMT
PLA/PBAT/0.6 ODA-MMT
PLA/PBAT/1.0 ODA-MMT
PLA/PBAT/3.0 ODA-MMT
The G” as the function of temperature for PLA/PBAT/ODA-MMT
66. Tg at different clay loading
Sample Identification Tg PLA (o
C) Tg PBAT (o
C)
PLA/PBAT 68.1 -23.0
PLA/PBAT/0.1 Na-MMT
PLA/PBAT/0.3 Na-MMT
PLA/PBAT/0.6 Na-MMT
PLA/PBAT/1.0 Na-MMT
PLA/PBAT/3.0 Na-MMT
57.6
59.3
59.8
64.3
60.8
-14.6
-10.7
-15.1
-10.1
-14.2
PLA/PBAT/0.1ODA-MMT
PLA/PBAT/0.3ODA-MMT
PLA/PBAT/0.6ODA-MMT
PLA/PBAT/1.0ODA-MMT
PLA/PBAT/3.0ODA-MMT
59.9
65.4
63.2
62.3
58.3
-15.1
-14.6
-9.6
-15.5
-13.6
67. 0
20
40
60
80
100
200 250 300 350 400 450 500 550
Temperature (o
C)
Weight%(%)
(a)
(b)
(c)
(d)
TGA thermograms of PLA/PBAT/Na-MMT (a) 0.3 wt% (b) 1.0 wt% and
(c) 3.0 wt% of Na-MMT
68. 0
20
40
60
80
100
200 250 300 350 400 450 500 550
Temperature (o
C)
Weight%(%)
(a)
(b) (c)
(d)
TGA thermograms of (a) PLA/PBAT, PLA/PBAT/ODA-MMT (b) 0.3 wt%
(c) 1.0 wt% and (d) 3.0 wt% of ODA-MMT
69. -22
-17
-12
-7
-2
200 250 300 350 400 450 500 550
Temperature (o
C)
DerivativesWeight%(%/m)
(a)
(b)
(c)
(d)
DTG thermograms of (a) PLA/PBAT, PLA/PBAT/Na-MMT (b) 0.3 wt%,
(c) 1.0 wt% and (d) 3.0 wt% of Na-MMT
70. -22
-17
-12
-7
-2
200 250 300 350 400 450 500 550
Temperature (o
C)
DerivativesWeight%(%/m)
(a)
(b)
(c)
(d)
DTG thermograms of (a) PLA/PBAT, PLA/PBAT/ODA-MMT (b) 0.3 wt%
(c) 1.0 wt% and (d) 3.0 wt% of ODA-MMT
71. Thermal degradation for PLA/PBAT/Na-MMT and PLA/PBAT/ODA-MMT
with various clay content
Type of clay Clay content (wt
%)
Tonset
(o
C) T50
(°C) Tmax
(°C)
PLA/PBAT 0.0 275.39 318.78 321.52
Na-MMT 0.3 284.97 319.68 320.43
1.0 286.71 325.27 329.38
3.0 299.71 330.27 332.38
ODA-MMT 0.3 308.57 333.60 334.56
1.0 310.36 336.09 336.93
3.0 315.17 343.22 345.585
72. 0
0.5
1
1.5
0 2 4 6 8 10 12 14 16 18
Time (days)
Waterabsorption
percentage(%)
PLA/PBAT PLA/PBAT/0.6 Na-MMT
PLA/PBAT/1.0 Na-MMT PLA/PBAT/3.0 Na-MMT
Water absorption percentage of PLA/PBAT/Na-MMT at various clay loading
73. 0
0.5
1
1.5
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
Time (days)
Waterabsorption
percentage(%)
PLA/PBAT PLA/PBAT/0.6 ODA-MMT
PLA/PBAT/1.0 ODA-MMT PLA/PBAT/3.0 ODA-MMT
Water absorption percentage of PLA/PBAT/ODA-MMT at various clay loading
78. •Two types of organoclays (ODA-MMT and DDOA-MMT) were successfully prepared
through ion exchange technique from Na-MMT (FTIR, XRD, TGA and elemental
analyzer).
•PLA/PBAT blends at different PBAT content were successfully prepared using melt
blending technique (Tensile testing, FTIR, DMA, SEM, water absorption and
biodegradability).
•PLA/PBAT/composites/nanocomposites at different type of clay were successfully
prepared using melt blending technique (XRD, FTIR, tensile testing, DMA, TGA,
SEM, TEM, water absorption and biodegradability).
•PLA/PBAT/composites/nanocomposites at different clay content were successfully
prepared using melt blending technique (XRD, tensile testing, DMA, TGA, water
absorption and biodegradability).
Conclusion
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