Processing and Characterization of PET Composites Reinforced With Geopolymer Concrete Waste

Pereira, Ana Paula dos Santos; Silva, Marcelo Henrique Prado da; Lima, Édio Pereira; Paula, Andersan dos Santos; Tommasini, Flávio James

doi:10.1590/1980-5373-MR-2017-0734

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Articles • Mat. Res. 20 (Suppl 2) • 2017 • https://doi.org/10.1590/1980-5373-MR-2017-0734 copy

Processing and Characterization of PET Composites Reinforced With Geopolymer Concrete Waste

Authorship SCIMAGO INSTITUTIONS RANKINGS

In the present study, poly (ethylene terephthalate)-based composites were produced and characterized. These composites were composed by poly (ethylene terephthalate) (PET) reinforced with geopolymer concrete waste (GCW). Both untreated (U-GCW) and treated with oleic acid (OA) geopolymer concrete waste (T-GCW) were used in the production of the composites. The PET/GCW ratios used for either treated or untreated GCW bodies were 80/20 (wt%), 60/40 (wt%) and 50/50 (wt%). Chemical compositions were assessed by X-ray fluorescence spectroscopy (XRF), crystallinity by differential scanning calorimetry (DSC), thermal stability by thermogravimetry (TGA), microstructure by field emission gun scanning electron microscopy (FEG-SEM) with energy dispersive X-ray spectroscopy (EDS), and mechanical properties were assessed by compression tests. Fourier transform infrared spectroscopy (FT-IR) was used to check the efficiency of the treatment with OA, as well as the interaction between PET and GCW. The T-GCW PET composites showed better thermal, physical, and mechanical properties, for non-structural applications, when compared to U-GCW.

Keywords:
PET composites; geopolymer concrete waste; poly (ethylene terephthalate); oleic acid; melt processing

Quantitative Results
Analyte	Content (%)	Analyte	Content (%)
SiO₂	46.708	TiO₂	0.903
CaO	24.419	MnO	0.180
Al₂O₃	14.362	SrO	0.094
K₂O	4.355	ZrO₂	0.085
Fe₂O₃	3.829	Rb₂O	0.015
SO₃	2.768	ZnO	0.013
MgO	2.274	Y₂O₃	0.005

Absorption bands (cm^-1)	Bands
3432	OH group (hydroxyl) ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.^,²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
3054	Symmetrical stretch of CH ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
2969 and 2908	C-H, Symmetrical stretching²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
2350	Axial symmetrical deformation of CO₂²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
1730	Stretching of C=O of carboxylic acid group ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.
1577 and 1504	Vibrations aromatic skeleton with stretching C=C ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.
1453, 1410 and 1342	Stretching of the C-O group deformation of the O-H group ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.^,²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998. and bending and wagging vibrational modes of the ethylene glycol segment ²¹21 Chen Z, Hay JN, Jenkins MJ. The thermal analysis of poly(ethylene terephthalate) by FTIR spectroscopy. Thermochimica Acta. 2013;552:123-130.
1240 and 1124	Terephthalate Group (OOCC₆H₄-COO) ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.
1096 and 1050	Methylene group ²¹21 Chen Z, Hay JN, Jenkins MJ. The thermal analysis of poly(ethylene terephthalate) by FTIR spectroscopy. Thermochimica Acta. 2013;552:123-130. and vibrations of the ester C-O bond ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
972, 872 and 848	Aromatic rings 1,2,4,5; Tetra replaced ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.^,²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
1960 and 795	Vibrations of adjacent two aromatic H in p-substituted compounds ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.^,²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998. and aromatic bands ²¹21 Chen Z, Hay JN, Jenkins MJ. The thermal analysis of poly(ethylene terephthalate) by FTIR spectroscopy. Thermochimica Acta. 2013;552:123-130.
712	Interaction of polar ester groups and benzene rings ¹⁹19 Edge M, Wiles R, Allen NS, McDonald WA, Mottock SV. Characterization of the species responsible for yellowing in melt degraded aromatic polyesters-I: Yellowing of poly(ethylene terephthalate). Polymer Degradation and Stability. 1996;53(2):141-151.

Absorption bands (cm^-1)	Bands
3447	O-H, stretch ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.^,²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³⁴34 Yang K, Peng H, Wen Y, Li N. Re-examination of characteristic FTIR spectrum of secondary layer in bilayer oleic acid-coated Fe3O4 nanoparticles. Applied Surface Science. 2010;256(10):3093-3097.
2516, 2348 and 1796	C=O; calcite, CaCO₃²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.
1640	Stretching vibration of O-H ³¹31 Ren X. Complete Recycling and Utilization of Waste Concrete Through Geopolymerization. [Dissertation]. Tucson: Department of Civil Engineering And Engineering Mechanics, The University of Arizona; 2015. 203 f.
1423	Stretching C=O ²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71. and O-H ²⁸28 Greco A, Maffezzoli A, Manni O. Development of polymeric foams from recycled polyethylene and recycled gypsum. Polymer Degradation and Stability. 2005;90(2):256-263.
1000	Si–O; silicate, C-S-H ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.^,²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³⁰30 Allahverdi A, Najafi Kani E. Construction Wastes as Raw Materials for Geopolymer Binders. International Journal of Civil Engineering. 2009;7(3):154-160.^,³¹31 Ren X. Complete Recycling and Utilization of Waste Concrete Through Geopolymerization. [Dissertation]. Tucson: Department of Civil Engineering And Engineering Mechanics, The University of Arizona; 2015. 203 f.
874	C-O, calcite, CaCO₃²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,²⁹29 Chollet M, Horgnies M. Analyses of the surfaces of concrete by Raman and FT-IR spectroscopies: comparative study of hardened samples after demoulding and after organic post-treatment. Surface and Interface Analysis. 2011;43(3):714-725.
796	Si-O-Si, symmetrical stretching ³²32 Springfield T. Application of FTIR for Quantification of Alkali in Cement. [Thesis]. Denton: University of North Texas; 2011. 58 f.^,³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.
713	CO₃, stretching ³²32 Springfield T. Application of FTIR for Quantification of Alkali in Cement. [Thesis]. Denton: University of North Texas; 2011. 58 f.
534	Si–O–Si out of plane bending mode ³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.
461	Si-O, stretching ³²32 Springfield T. Application of FTIR for Quantification of Alkali in Cement. [Thesis]. Denton: University of North Texas; 2011. 58 f.

Absorption bands (cm^-1)	Bands
3440	O-H, stretch ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.^,²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³⁴34 Yang K, Peng H, Wen Y, Li N. Re-examination of characteristic FTIR spectrum of secondary layer in bilayer oleic acid-coated Fe3O4 nanoparticles. Applied Surface Science. 2010;256(10):3093-3097.
2924, 2852, 1578 and 1541	Group vibrations CH ¹³13 Ramos FJHTV, Mendes LC, Cestari SP. Organically modified concrete waste with oleic acid. Journal of Thermal Analysis and Calorimetry. 2015;119(3):1895-1904. and CH₂³⁴34 Yang K, Peng H, Wen Y, Li N. Re-examination of characteristic FTIR spectrum of secondary layer in bilayer oleic acid-coated Fe3O4 nanoparticles. Applied Surface Science. 2010;256(10):3093-3097.
2360 and 2342	Symmetric axial deformation of the CO₂²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.
1736	Stretching vibration of O-H ³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.
1468	C=O e OH, stretching and CH₂ Vibrational deformation³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.^,³⁴34 Yang K, Peng H, Wen Y, Li N. Re-examination of characteristic FTIR spectrum of secondary layer in bilayer oleic acid-coated Fe3O4 nanoparticles. Applied Surface Science. 2010;256(10):3093-3097.
1420	C=O e OH, stretching ²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,²⁹29 Chollet M, Horgnies M. Analyses of the surfaces of concrete by Raman and FT-IR spectroscopies: comparative study of hardened samples after demoulding and after organic post-treatment. Surface and Interface Analysis. 2011;43(3):714-725.
1091	Si–O–Si asymmetric stretching vibration ²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³⁰30 Allahverdi A, Najafi Kani E. Construction Wastes as Raw Materials for Geopolymer Binders. International Journal of Civil Engineering. 2009;7(3):154-160.^,³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.
1004	Si–O; silicate, C-S-H ²⁰20 Silverstein RM, Webster FX. Spectrometric Identification of Organic Compounds. New York: Wiley; 1998.^,²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³¹31 Ren X. Complete Recycling and Utilization of Waste Concrete Through Geopolymerization. [Dissertation]. Tucson: Department of Civil Engineering And Engineering Mechanics, The University of Arizona; 2015. 203 f.
874	C-O, calcite, CaCO₃²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,²⁹29 Chollet M, Horgnies M. Analyses of the surfaces of concrete by Raman and FT-IR spectroscopies: comparative study of hardened samples after demoulding and after organic post-treatment. Surface and Interface Analysis. 2011;43(3):714-725.
669	Si-O bending ²²22 Piqué TM, Vázquez A. Uso de Espectroscopia Infrarroja con Transformada de Fourier (FTIR) en el estudio de la hidratación del cemento. Concreto y cimento. Investigación y Desarrollo. 2012;3(2):62-71.^,³²32 Springfield T. Application of FTIR for Quantification of Alkali in Cement. [Thesis]. Denton: University of North Texas; 2011. 58 f.
465	O-Si-O, bending vibration ³²32 Springfield T. Application of FTIR for Quantification of Alkali in Cement. [Thesis]. Denton: University of North Texas; 2011. 58 f.^,³³33 Tantawy MA, Shatat MR, El-Roudi AM, Taher MA, Abd-El-Ramed M. Low Temperature Synthesis of Belite Cement Based on Silica Fume and Lime. International Scholarly Research Notices. 2014;2014:873215.

Samples	T_onset1 (ºC)	T_max1 (ºC)	T_end1 (ºC)	T_onset2 (ºC)	T_max2 (ºC)	T_end2 (ºC)	T_onset3 (ºC)	T_max3 (ºC)	T_end3 (ºC)	Residues (%)
PET	374	434	468	---	---	---	---	---	---	11
U-GCW	45	60	71	389	422	431	591	667	685	82
T-GCW	46	77	108	374	447	508	616	672	686	74
PET/U-GCW 50/50	335	431	470	526	577	614	664	684	696	56
PET/U-GCW 60/40	358	435	471	537	573	603	642	667	690	49
PET/U-GCW 80/20	350	437	482	548	583	615	----	----	----	34
PET/T-GCW 50/50	347	426	478	534	573	597	654	683	695	52
PET/T-GCW 60/40	350	434	474	533	574	600	655	680	696	40
PET/T-GCW 80/20	351	435	492	530	574	616	----	----	----	31

Samples	T_m(ºC)	T_c(ºC)	ΔH_m(J/g)	ΔH_c (J/g)	X_c (%)
PET	246.25	199.03	44.21	45.20	31.58
50/50 PET/U-GCW	239.04	162.72	1.72	0.80	2.46
60/40 PET/ U-GCW	244.33	171.91	9.50	6.25	11.31
80/20 PET/ U-GCW	252.08	200.54	28.87	25.67	25.78
50/50 PET/T-GCW	223.30	107.30	0.28	0.34	0.40
60/40 PET/ T-GCW	229.15	163.09	5.82	5.78	6.93
80/20 PET/ T-GCW	246.44	204.71	26.43	23.56	23.60

Samples	Compressive strength (MPa)
50/50 PET/ U-GCW	1.86 ± 0.51
60/40 PET/ U-GCW	1.32 ± 0.29
80/20 PET/ U-GCW	1.23 ± 0.49
50/50 PET/ T-GCW	2.46 ± 0.62
60/40 PET/ T-GCW	2.38 ± 0.50
80/20 PET/ T-GCW	1.46 ± 0.43

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