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Frontiers of Chemical Science and Engineering

ISSN 2095-0179

ISSN 2095-0187(Online)

CN 11-5981/TQ

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Front Chem Sci Eng    2012, Vol. 6 Issue (4) : 395-402    https://doi.org/10.1007/s11705-012-1269-2
RESEARCH ARTICLE
Dispersion of a novel phenolic rigid organic filler in isotactic polypropylene matrix by solution-mixing and melt-mixing
Dongming QI(), Xiaoli ZHAO, Zhijie CHEN, Peng HUANG, Jun CAO
Key Laboratory of Advanced Textile Materials and Manufacturing Technology (Ministry of Education), Zhejiang Sci-Tech University, Hangzhou 310018, China
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Abstract

A novel phenolic rigid organic filler (named KD) with a high melting point was dispersed in an isotactic polypropylene (iPP) matrix by solution-mixing and/or melt-mixing. A series of KD/iPP blends was prepared with or without addition of maleic anhydride-grafted polypropylene (MAPP) as a compatibilizer. Influences of MAPP and mixing methods on the filler dispersion were studied using polaried optical microscope (POM), scanning electron microscope (SEM) and tensile test. The filler particles are always inclined to form large irregular aggregates in the iPP matrix due to their significant differences in polarity and solubility in solvent. However, an iPP/MAPP/KD (PMK) blend containing filler particles with a quasi-spherical shape (~97.8 nm in diameter) and narrow particle size distribution (polydispersity index= 1.076) was successfully prepared by incorporating MAPP to reduce the interfacial tension and surface free energy between the dispersion phase and the continuous phase, and adopting a spray-drying method after solution-mixing to suppress the increase of the size of the dispersed phase during the removal of solvent.
Keywords dispersion      rigid organic filler      isotactic polypropylene      mixing     
Corresponding Author(s): QI Dongming,Email:dongmingqi@zstu.edu.cn   
Issue Date: 05 December 2012
 Cite this article:   
Dongming QI,Xiaoli ZHAO,Zhijie CHEN, et al. Dispersion of a novel phenolic rigid organic filler in isotactic polypropylene matrix by solution-mixing and melt-mixing[J]. Front Chem Sci Eng, 2012, 6(4): 395-402.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-012-1269-2
https://academic.hep.com.cn/fcse/EN/Y2012/V6/I4/395
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
Fig.1  Chemical structure of the phenolic rigid organic filler (KD)
No.Mixing methodSamplesFiller /%MAPP /%Spray-drying
1Melt-mixing*PK15.00Not used
2PMK15.01.3Not used
3PMK25.05.0Not used
4Solution-mixingPP00Used
5PM05.0Used
6PK25.00Not used
7PK35.00Used
8PMK35.05.0Not used
9PMK40.55.0Used
10PMK52.55.0Used
11PMK65.05.0Used
12PMK710.05.0Used
13Solution-mixing*+ Melt-mixingPK45.00Used
14PMK85.05.0Used
Tab.1  Process conditions and components for the preparation of iPP(PP), iPP/MAPP(PM), iPP/KD(PK), and iPP/MAPP/KD(PMK) blends
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.2  SEM micrographs of the filler powder (KD) with different magnifications
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.3  POM micrographs of iPP/KD blends heated at (a) 220°C and (b) 270°C (200 × )
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.4  POM micrographs of PK and PMK blends (filler content: 5%) observed in a hot stage at 180°C. The blends were prepared by melt-mixing in a twin-screw mixer and the magnifications were 200
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.5  POM micrographs of PK and PMK blends observed in a hot stage at 180°C. (a) PK2 blend prepared by solution-mixing without spray-drying; (b) PK3 blend prepared by solution-mixing using spray-drying; (c) PK4 blend prepared by further melt-mixing of the PK3 blend; (d) PMK3 blend prepared by solution-mixing without spray-drying; (e) PMK6 blend prepared by solution-mixing using spray-drying; (f) PMK8 blend prepared by further melt-mixing of the PMK6 blend
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.6  The solubility of iPP and KD in xylene at different temperatures
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.7  Typical SEM micrographs of the cryogenically fractured surfaces of (a) PP blend, (b) and (c) PMK6 blend at different magnifications
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.8  The filler particle size distribution in the PMK6 blend, counted from the SEM micrographs in Fig. 7
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
Fig.9  Typical tensile curves of PK and PMK specimens under fixed filler content
No.SamplesYoung’s modulus /MPaYield pointBreak point
Strain /%Stress /MPaStrain /%Stress /MPa
1PP83412.833.83108544.9
2PK188912.235.721833.1
3PMK287512.734.9441227.5
4PK28928.131.5931.4
5PK39539.230.92020.8
6PMK6104212.335.8247828.9
Tab.2  The tensile properties of PP, PK and PMK sheets at a crosshead speed of 10 mm·min
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