scholarly journals Rheological behaviour of thermoplastic poly(ester-siloxane)s

2010 ◽  
Vol 64 (6) ◽  
pp. 537-545 ◽  
Author(s):  
Vesna Antic ◽  
Marija Pergal ◽  
Malisa Antic ◽  
Jasna Djonlagic
Keyword(s):  
Dynamic Viscosity ◽  
Microphase Separation ◽  
Soft Segment ◽  
Rheological Behaviour ◽  
Thermoplastic Elastomers ◽  
Degree Of Crystallinity ◽  
Mass Ratio ◽  
Complex Dynamic ◽  
Constant Length ◽  
Soft Segments

Two series of thermoplastic elastomers (TPES) based on poly(dimethylsiloxane), (PDMS) as the soft segment and poly(butylene terephthalate) (PBT) as the hard segment, were analyzed by dynamic mechanical spectroscopy. In the first TPES series the lengths of both hard and soft segments were varied while the mass ratio of the hard to soft segments was nearly constant (about 60 mass%). In the second series, the mass ratio of hard and soft segments was varied in the range from 60/40 to 40/60, with a constant length of soft PDMS segments. The influence of the structure and composition of TPESs on the rheological properties, such as complex dynamic viscosity, ?*, the storage, G?, and loss, G?, shear modulus as well as the microphase separation transition temperature, TMST, was examined. The obtained results showed that the storage modulus of the TPESs increased in a rubbery plateau region with increasing degree of crystallinity. The rheological measurements of TPESs also showed that a microphase reorganization occurred during the melting process. The microphase separation transition temperatures were in the range from 220 to 234 ?C. In the isotropic molten state, the complex dynamic viscosity increased with increasing both the content and lenght of hard PBT segments.

scholarly journals Impact of Macrodiols on the Morphological Behavior of H12MDI/HDO-Based Polyurethane Elastomer

Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2060
Author(s):  
Shazia Naheed ◽  
Mohammad Zuber ◽  
Mahwish Salman ◽  
Nasir Rasool ◽  
Zumaira Siddique ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Contact Angle ◽  
Chain Length ◽  
Microphase Separation ◽  
Soft Segment ◽  
Group Identification ◽  
Degree Of Crystallinity ◽  
Polyurethane Elastomers ◽  
Hard Segments ◽  
Morphological Behavior

In this study, we evaluated the morphological behavior of polyurethane elastomers (PUEs) by modifying the soft segment chain length. This was achieved by increasing the soft segment molecular weight (Mn = 400–4000 gmol−1). In this regard, polycaprolactone diol (PCL) was selected as the soft segment, and 4,4′-cyclohexamethylene diisocyanate (H12MDI) and 1,6-hexanediol (HDO) were chosen as the hard segments. The films were prepared by curing polymer on Teflon surfaces. Fourier transform infrared spectroscopy (FTIR) was utilized for functional group identification in the prepared elastomers. FTIR peaks indicated the disappearance of −NCO and −OH groups and the formation of urethane (NHCOO) groups. The morphological behavior of the synthesized polymer samples was also elucidated using scanning electron microscopy (SEM) and atomic force microscopy (AFM) techniques. The AFM and SEM results indicated that the extent of microphase separation was enhanced by an increase in the molecular weight of PCL. The phase separation and degree of crystallinity of the soft and hard segments were described using X-ray diffraction (XRD). It was observed that the degree of crystallinity of the synthesized polymers increased with an increase in the soft segment’s chain length. To evaluate hydrophilicity/hydrophobicity, the contact angle was measured. A gradual increase in the contact angle with distilled water and diiodomethane (38.6°–54.9°) test liquids was observed. Moreover, the decrease in surface energy (46.95–24.45 mN/m) was also found to be inconsistent by increasing the molecular weight of polyols.

scholarly journals Synthesis of thermoplastic poly(ester-olefin) elastomers

2004 ◽  
Vol 58 (10) ◽  
pp. 444-449
Author(s):  
Branka Tanasijevic ◽  
Salem Elkhaseh ◽  
Marija Nikolic ◽  
Jasna Djonlagic
Keyword(s):  
Soft Segment ◽  
Weight Ratio ◽  
Soxhlet Extraction ◽  
Thermoplastic Elastomers ◽  
Molecular Structures ◽  
Degree Of Crystallinity ◽  
Molar Ratio ◽  
Mechanical Spectroscopy ◽  
Scanning Calorimetry ◽  
High Boiling Solvent

A series of thermoplastic poly(ester-olefin) elastomers, based on poly(ethylene-stat-butylene), HO-PEB-OH, as the soft segment and poly (butylene terephthalate), PBT, as the hard segment, were synthesized by a catalyzed transesterification reaction in solution. The incorporation of soft hydrogenated poly(butadiene) segments into the copolyester backbone was accomplished by the polycondensation of ?, ?-dihydroxyl telechelic HO-PEB-OH, (PEB Mn = 3092 g/mol) with 1,4-butanediol (BD) and dimethyl terephthalate (DMT) in the presence of a 50 wt-% high boiling solvent i.e., 1,2,4-trichlorobenzene. The molar ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 60:40. The synthesis was optimized in terms of both the concentration of catalyst, tetra-n-butyl-titanate (Ti(OBu)4), and stabilizer, N,N'-diphenyl-p-phenylenediamine (DPPD), as well as the reaction time. It was found that the optimal catalyst concentration (Ti(OBu)4) for the synthesis of these thermoplastic elastomers was 1.0 mmol/mol ester and the optimal DPPD concentration was 1.0 wt-%. The extent of the reaction was followed by measuring the inherent viscosity of the reaction mixture. The effectiveness of the incorporation of the soft segments into the copolymer chains was proved by Soxhlet extraction with chloroform. The molecular structures, composition and the size of the synthesized poly(ester-butylene)s were verified by 1H NMR spectroscopy, viscometry of dilute solutions and the complex dynamic melt viscosity. The thermal properties of poly(ester-olefin)s were investigated by differential scanning calorimetry (DSC). The degree of crystallinity was also determined by DSC. The thermal and thermo-oxidative stability were investigated by thermogravimetric analysis (TGA). The rheological properties of poly(ester-olefin)s were investigated by dynamic mechanical spectroscopy in the melt and solid state.

Study on the Influences of Domain Structure of Hydrophilic Polyurethane with Partially Crystalline on its Moisture Permeability

2011 ◽  
Vol 233-235 ◽  
pp. 281-287
Author(s):  
Heng Quan ◽  
Zhen Ya Gu
Keyword(s):  
Chemical Structure ◽  
Hard Segment ◽  
Microphase Separation ◽  
Soft Segment ◽  
Moisture Permeability ◽  
Soft Segments ◽  
Separation Degree ◽  
Polyethylene Glycol 1000 ◽  
Segmented Polyurethanes ◽  
Hydrophilic Polyurethane

Multiphase, segmented polyurethanes with mixed soft segment phase were prepared from 4,4’- diphenylmethane diisocyanate (Pure MDI), polybutylene adipate (glycol) 2000 (PBA2000) and polyethylene glycol 1000 (PEG1000) with 1,4-butanediol (BDO) as the chain extender. Further more, the relationships between domain separation structure, crystallizability of soft segment and moisture permeability, hydrophilic property, phase inversion temperature (PIT) of the polyurethanes were investigated. The studies show that the chemical structure, concentration of hydrophilic soft monomers and the microphase separation degree of the mixed soft segments from hard segment domain have remarkable effects on the application properties of polyurethane.

scholarly journals Synthesis, structure and properties of thermoplastic poly(ester-siloxane) elastomers

2006 ◽  
Vol 71 (7) ◽  
pp. 839-842
Author(s):  
Vesna Antic ◽  
Jasna Djonlagic
Keyword(s):  
1H Nmr Spectroscopy ◽  
Mechanical Analysis ◽  
Structure And Properties ◽  
Mass Ratio ◽  
Scanning Calorimetry ◽  
Constant Length ◽  
Melting Temperatures ◽  
Soft Segments ◽  
In Series ◽  
Hard Segments

Two series of thermoplastic poly(ester-siloxane) elastomers (TPES), with hard segments based on poly(butylene terephthalate) (PBT) and soft segments based on poly(dimethylsiloxane) (PDMS), were synthesized by high-temperature two-step transesterification reaction in the melt. In series I, the mass ratio of hard and soft segments was kept constant (57:43), while the length of the segments was varied, whereas in series II, the mass ratio of hard and soft segments was varied in range from 70:30 to 40:60, with a constant length of the soft segments. The segmented structure of the poly(ester-siloxane) copolymers was verified by 1H-NMR spectroscopy of the soluble and insoluble fractions, obtained after extraction of the samples with chloroform. The influence of the structure and composition of the TPES on the melting temperatures and degrees of crystallinity was investigated by differential scanning calorimetry (DSC). The rheological properties were investigated by dynamic mechanical analysis (DMA).

scholarly journals Structural, thermal and surface characterization of thermoplastic polyurethanes based on poly(dimethylsiloxane)

2014 ◽  
Vol 79 (7) ◽  
pp. 843-866 ◽  
Author(s):  
Marija Pergal ◽  
Ivan Stefanovic ◽  
Dejan Godjevac ◽  
Vesna Antic ◽  
Vesna Milacic ◽  
...  
Keyword(s):  
Surface Properties ◽  
Surface Characterization ◽  
Soft Segment ◽  
Hydrophobic Surface ◽  
Sem Analysis ◽  
Degree Of Crystallinity ◽  
Water Contact ◽  
Thermoplastic Polyurethanes ◽  
Melting Temperatures ◽  
Soft Segments

In this study, the synthesis, structure and physical properties of two series of thermoplastic polyurethanes based on hydroxypropyl terminated poly(dimethylsiloxane) (HP-PDMS) or hydroxyethoxy propyl terminated poly(dimethylsiloxane) (EO-PDMS) as a soft segment, and 4,4?-methylenediphenyl diisocyanate and 1,4-butanediol as a hard segment were investigated. Each series is composed of samples prepared with a different soft segment. The polyurethanes were synthesized by two-step polyaddition in solution. The effects of the type and content of PDMS segments on the structure, thermal and surface properties of copolymers were studied by 1H NMR, 13C NMR and two-dimensional NMR (HMBC and ROESY) spectroscopy, GPC, DSC, TGA, WAXS, SEM, water contact angle and water absorption measurements. Thermal properties investigated by DSC indicated that the presence of soft PDMS segments lowers the glass transition and melting temperatures of the hard phase as well as the degree of crystallinity. SEM analysis of copolymers with a lower soft segment content confirmed the presence of spherulite superstructures, which arise from the crystallization of the hard segments. When compared with polyurethanes prepared from HP-PDMS, copolymers synthesized from EO-PDMS with the same content of the soft segments have higher degree of crystallinity, better thermal stability and less hydrophobic surface. Our results show that the synthesized polyurethanes have good thermal and surface properties, which could be further modified by changing the type or content of the soft segments.

scholarly journals Synthesis of thermoplastic poly(ester-siloxane)s in the melt and in solution

2005 ◽  
Vol 70 (12) ◽  
pp. 1469-1485 ◽  
Author(s):  
Biljana Dojcinovic ◽  
Vesna Antic ◽  
Marija Vuckovic ◽  
Jasna Djonlagic
Keyword(s):  
1H Nmr Spectroscopy ◽  
Hard Segment ◽  
Soft Segment ◽  
Weight Ratio ◽  
Thermoplastic Elastomers ◽  
Degree Of Crystallinity ◽  
Mechanical Spectroscopy ◽  
Scanning Calorimetry ◽  
Melting Temperatures ◽  
High Boiling Solvent

Two series of thermoplastic elastomers, based on poly(dimethylsiloxane) PDMS, as the soft segment and poly(butylene terephthalate), PBT, as the hard segment, were synthesized by catalyzed transesterification, from dimethyl terephthalate, DMT, silanol-terminated poly(dimethylsiloxane), PDMS-OH Mn=1750g/mol, and 1,4-butanediol, BD. The mole ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 55:45. The first series was synthesized in order to determine the optimal mole ratio of BD and DMT for the synthesis of high molecular weight thermoplastic poly(ester-siloxane)s, TPESs. The second series was performed in the presence of the high-boiling solvent, 1,2,4-trichlorbenzene in order to increase the mixing between the extremely non-polar siloxane prepolymer and the polar reactants, DMT and BD, and, therefore, avoid phase separation during synthesis. The structure and composition of the synthesized poly(ester-siloxane)s were verified by 1H-NMR spectroscopy, while the melting temperatures and degree of crystallinity were determined by differential scanning calorimetry (DSC). The effectiveness of the incorporation of the silanol-terminated poly( dimethylsiloxane) into the polyester chains was verified by chloroform extraction. The rheological properties of the poly(ester-siloxane)s were investigated by dynamic mechanical spectroscopy (DMA).

scholarly journals Determination of rheological behaviour of wine lees

2015 ◽  
Vol 29 (3) ◽  
pp. 307-311 ◽  
Author(s):  
Jaromír Lachman ◽  
Kazimierz Rutkowski ◽  
Petr Trávníček ◽  
Tomáš Vítěz ◽  
Patrik Burg ◽  
...  
Keyword(s):  
Dynamic Viscosity ◽  
Rheological Behaviour ◽  
Volatile Acid ◽  
Second Phase ◽  
Temperature Hysteresis ◽  
Chemical Background ◽  
Rate Test ◽  
Red Grape ◽  
Increasing Temperature

Abstract This study deals with the rheological properties of wine lees. Samples of wine lees of the Saint Laurent variety were used in this experiment. The investigated wine lees arose in the process of production red grape wine in 2013 (Czech Republic). At first, the chemical background was determined. The chemical background includes the following chemical parameters: total acidity, pH, alcohol content, reduced sugars, free SO2, total SO2, and volatile acid. In the second phase of the study, physical properties were determined. Specifically, a sample of wine lees was subjected to rheological tests. These tests consisted in determination of dependence of dynamic viscosity on the temperature, hysteresis loop tests, dependence of dynamic viscosity on the time and step-down in the shear rate test. The experiment demonstrated that the dynamic viscosity increased with increased temperature – this phenomenon is caused by thermolabile proteins – and the wine lees has rheopectic behaviour; the degree of rheopexy was found to rise with the increasing temperature.

scholarly journals Studies of the Sulfonated Hydrogenated Styrene–Isoprene–Styrene Block Copolymer and Its Surface Properties, Cytotoxicity, and Platelet-Contacting Characteristics

Polymers ◽  
2021 ◽  
Vol 13 (2) ◽  
pp. 235
Author(s):  
Bin-Hong Tsai ◽  
Tse-An Lin ◽  
Chi-Hui Cheng ◽  
Jui-Che Lin
Keyword(s):  
Block Copolymer ◽  
Biomedical Applications ◽  
Human Life ◽  
Thermoplastic Elastomers ◽  
Wound Dressings ◽  
Tert Butyl ◽  
Soft Segments ◽  
Good Biocompatibility ◽  
Uv Ozone ◽  
Ozone Resistance

Styrenic thermoplastic elastomers (TPEs) consist of styrenic blocks. They are connected with other soft segments by a covalent linkage and are widely used in human life. However, in biomedical applications, TPEs need to be chemically hydrogenated in advance to enhance their properties such as strong UV/ozone resistance and thermal-oxidative stability. In this study, films composed of sulfonated hydrogenated TPEs were evaluated. Hydrogenated tert-butyl styrene–styrene–isoprene block copolymers were synthesized and selectively sulfonated to different degrees by reaction with acetyl sulfate. By controlling the ratio of the hydrogenated tert-butyl styrene–styrene–isoprene block copolymer and acetyl sulfate, sulfonated films were optimized to demonstrate sufficient mechanical integrity in water as well as good biocompatibility. The thermal plastic sulfonated films were found to be free of cytotoxicity and platelet-compatible and could be potential candidates in biomedical film applications such as wound dressings.

Effect of Block Molecular Weight on the Mechanical Properties of PA1010-b-PEG Segmented Block Copolymers

2012 ◽  
Vol 512-515 ◽  
pp. 2127-2130
Author(s):  
Li Huo ◽  
Cai Xia Dong
Keyword(s):  
Mechanical Properties ◽  
Molecular Weight ◽  
Block Copolymers ◽  
Microphase Separation ◽  
Soft Segment ◽  
Mechanical Measurements ◽  
Wide Range ◽  
Hard Block ◽  
Higher Temperature ◽  
Hard Segments

The mechanical properties were investigated of a series of PA-PEG thermalplastic elastomer based on PA1010 and polytetramethylene glycol (PEG) with varying hard and soft segment content. Dynamic mechanical measurements of these polymers have carried out over a wide range of temperatures. The block copolymers exhibit three peaks, designated as α, β and γ in the tanδ-temperature curve. The α transition shifts to higher temperature with increasing hard block molecular weight. However, at a constant hard molecular weight, the α transition shifts to higher temperature and the damping increases on increasing the soft segment molecular weight. DMA results show that the block copolymers exhibit a microphase separation structure and both soft and hard segments were found to be crystallizable. The degree of phase separation increases with increasing hard block molecular weight.

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