Vitrimerization of Poly(butylene succinate) By Reactive Melt Mixing Using Zn(II) Epoxy-Vitrimer Chemistry

2021 ◽  
Vol 7 (1) ◽  
pp. 10
Author(s):  
Christos Panagiotopoulos ◽  
Dimitrios Korres ◽  
Stamatina Vouyiouka
Keyword(s):  
Dynamic Network ◽  
Research Programme ◽  
Basic Research ◽  
Diglycidyl Ether ◽  
Exchange Reactions ◽  
Melt Mixing ◽  
Vacuum Oven ◽  
Butylene Succinate ◽  
Polymer Backbone ◽  
Reactive Melt

Vitrimers constitute a new class of covalent adaptable networks (CANs), in which thermally stimulated associative exchange reactions allow the topological rearrangement of the dynamic network while keeping the number of bonds and the crosslink density constant. The current study proposed a solvent-free method to synthesize vitrimers by reactive melt mixing using a commercial biobased/biodegradable polyester, poly(butylene succinate), PBS. More specifically, a two-step process was followed; the first step involved reactive mixing of PBS with the crosslinker (diglycidyl ether of bisphenol A, DGEBA) and the transesterification catalyst (Zinc(II) acetylacetonate hydrate, Zn(acac)2) in a twin-screw mini-compounder, in order to incorporate the epoxy groups in the polymer backbone. The second step (vitrimerization) comprised a crosslinking process of the homogenous mixtures in a vacuum oven at 170 °C, resulting in the formation of a dynamic crosslinked network with epoxy moieties serving as the crosslinkers. By tuning the crosslinker content (0–10% mol with respect to PBS repeating unit) and the Zinc(II) catalyst to crosslinker ratio (0 to 1), tailor-made vitrimers were prepared with high insolubility and improved melt strength. Moreover, PBS vitrimers could still be reprocessed by compression molding after the crosslinking, which enables the recycling process. This work was made possible by the “Basic Research Programme, NTUA, PEVE 2020 NTUA” [PEVE0050] of the National Technical University of Athens and is gratefully acknowledged.

scholarly journals Peroxide-Induced Synthesis of Maleic Anhydride-Grafted Poly(butylene succinate) and Its Compatibilizing Effect on Poly(butylene succinate)/Pistachio Shell Flour Composites

Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5927
Author(s):  
Sandra Rojas-Lema ◽  
Jordi Arevalo ◽  
Jaume Gomez-Caturla ◽  
Daniel Garcia-Garcia ◽  
Sergio Torres-Giner
Keyword(s):  
Maleic Anhydride ◽  
Hydrogen Abstraction ◽  
Green Composites ◽  
Melt Mixing ◽  
Butylene Succinate ◽  
Oh Groups ◽  
Pistachio Shell ◽  
Reactive Melt ◽  
Reactive Compatibilizer ◽  
Compost Soil

Framing the Circular Bioeconomy, the use of reactive compatibilizers was applied in order to increase the interfacial adhesion and, hence, the physical properties and applications of green composites based on biopolymers and food waste derived lignocellulosic fillers. In this study, poly(butylene succinate) grafted with maleic anhydride (PBS-g-MAH) was successfully synthetized by a reactive melt-mixing process using poly(butylene succinate) (PBS) and maleic anhydride (MAH) that was induced with dicumyl peroxide (DCP) as a radical initiator and based on the formation of macroradicals derived from the hydrogen abstraction of the biopolymer backbone. Then, PBS-g-MAH was used as reactive compatibilizer for PBS filled with different contents of pistachio shell flour (PSF) during melt extrusion. As confirmed by Fourier transform infrared (FTIR), PBS-g-MAH acted as a bridge between the two composite phases since it was readily soluble in PBS and could successfully form new esters by reaction of its multiple MAH groups with the hydroxyl (–OH) groups present in cellulose or lignin of PSF and the end ones in PBS. The resultant compatibilized green composites were, thereafter, shaped by injection molding into 4-mm thick pieces with a wood-like color. Results showed significant increases in the mechanical and thermomechanical rigidity and hardness, meanwhile variations on the thermal stability were negligible. The enhancement observed was related to the good dispersion and the improved filler-matrix interfacial interactions achieved by PBS-g-MAH and also to the PSF nucleating effect that increased the PBS’s crystallinity. Furthermore, water uptake of the pieces progressively increased as a function of the filler content, whereas the disintegration in controlled compost soil was limited due to their large thickness.

Mechanical Property Improvement of Poly(Butylene Succinate) by Reinforcing with Modified Fumed Silica

2014 ◽  
Vol 1025-1026 ◽  
pp. 215-220 ◽  
Author(s):  
Sasirada Weerasunthorn ◽  
Pranut Potiyaraj
Keyword(s):  
Mechanical Properties ◽  
Tensile Strength ◽  
Impact Strength ◽  
Flexural Strength ◽  
Fumed Silica ◽  
Tensile Modulus ◽  
Silica Particles ◽  
Melt Mixing ◽  
Butylene Succinate ◽  
Ir Spectrophotometry

Fumed silica particles (SiO2) were directly added into poly (butylene succinate) (PBS) by melt mixing process. The effects of amount of fumed silica particles on mechanical properties of PBS/fumed silica composites, those are tensile strength, tensile modulus, impact strength as well as flexural strength, were investigated. It was found that the mechanical properties decreased with increasing fumed silica loading (0-3 wt%). In order to increase polymer-filler interaction, fumed silica was treated with 3-glycidyloxypropyl trimethoxysilane (GPMS), and its structure was analyzed by FT-IR spectrophotometry. The PBS/modified was found to possess better tensile strength, tensile modulus, impact strength and flexural strength that those of PBS/fumed silica composites.

scholarly journals GYNOCARE Update: Modern Strategies to Improve Diagnosis and Treatment of Rare Gynecologic Tumors—Current Challenges and Future Directions

Cancers ◽  
2021 ◽  
Vol 13 (3) ◽  
pp. 493
Author(s):  
Riccardo Di Fiore ◽  
Sherif Suleiman ◽  
Bridget Ellul ◽  
Sharon A. O’Toole ◽  
Charles Savona-Ventura ◽  
...  
Keyword(s):  
Cancer Research ◽  
Gynecological Cancer ◽  
Gynecologic Cancer ◽  
Delayed Diagnosis ◽  
Research Programme ◽  
Basic Research ◽  
Diagnosis And Treatment ◽  
Rare Cancer ◽  
Cost Action ◽  
Gynecologic Tumors

More than 50% of all gynecologic tumors can be classified as rare (defined as an incidence of ≤6 per 100,000 women) and usually have a poor prognosis owing to delayed diagnosis and treatment. In contrast to almost all other common solid tumors, the treatment of rare gynecologic tumors (RGT) is often based on expert opinion, retrospective studies, or extrapolation from other tumor sites with similar histology, leading to difficulty in developing guidelines for clinical practice. Currently, gynecologic cancer research, due to distinct scientific and technological challenges, is lagging behind. Moreover, the overall efforts for addressing these challenges are fragmented across different European countries and indeed, worldwide. The GYNOCARE, COST Action CA18117 (European Network for Gynecological Rare Cancer Research) programme aims to address these challenges through the creation of a unique network between key stakeholders covering distinct domains from concept to cure: basic research on RGT, biobanking, bridging with industry, and setting up the legal and regulatory requirements for international innovative clinical trials. On this basis, members of this COST Action, (Working Group 1, “Basic and Translational Research on Rare Gynecological Cancer”) have decided to focus their future efforts on the development of new approaches to improve the diagnosis and treatment of RGT. Here, we provide a brief overview of the current state-of-the-art and describe the goals of this COST Action and its future challenges with the aim to stimulate discussion and promote synergy across scientists engaged in the fight against this rare cancer worldwide.

Poly(Butylene Succinate) Composites Reinforced with Short Sisal Fibres

2001 ◽  
Vol 9 (5) ◽  
pp. 333-338 ◽  
Author(s):  
Mitsuhiro Shibata ◽  
Retsu Makino ◽  
Ryutoku Yosomiya ◽  
Hiroyuku Takeishi
Keyword(s):  
Mechanical Properties ◽  
Tensile Strength ◽  
Fibre Length ◽  
Mechanical Analysis ◽  
Fibre Content ◽  
Flexural Properties ◽  
Melt Mixing ◽  
Butylene Succinate ◽  
Sisal Fibre ◽  
The Matrix

Poly(butylene succinate) composites reinforced with short sisal fibre were prepared by melt mixing and subsequent injection moulding. The influence of fibre length, fibre content and the surface treatment of the natural fibres on the mechanical properties of the composites were evaluated. Regarding fibre length, the tensile and flexural properties of the composites had maxima at a fibre length of about 5 mm. The flexural and tensile moduli of the composites increased with increasing fibre content. Although the tensile strength hardly changed, the flexural strength increased up to a fibre content of 10 wt%. The dynamic mechanical analysis of the composites showed that the storage moduli at above ca.-16°C (corresponding to the glass transition temperature of the matrix) increased with increasing fibre content.

scholarly journals Effect of exchange reactions and free radical grafting on the high‐speed reactive extrusion of poly(butylene succinate) and poly(propylene carbonate) blends

2019 ◽  
Vol 59 (10) ◽  
pp. 1986-1998
Author(s):  
Bárbara A. Calderón ◽  
Conor W. Thompson ◽  
Vincenzo L. Barinelli ◽  
Matthew S. McCaughey ◽  
Margaret J. Sobkowicz
Keyword(s):  
Free Radical ◽  
Propylene Carbonate ◽  
High Speed ◽  
Reactive Extrusion ◽  
Exchange Reactions ◽  
Butylene Succinate ◽  
Poly Propylene

scholarly journals Enzymatic Degradation of Acrylic Acid-Grafted Poly(butylene succinate-co-terephthalate) Nanocomposites Fabricated Using Heat Pressing and Freeze-Drying Techniques

Materials ◽  
2020 ◽  
Vol 13 (2) ◽  
pp. 376 ◽  
Author(s):  
Sheng-Hsiang Lin ◽  
Hsiang-Ting Wang ◽  
Jie-Mao Wang ◽  
Tzong-Ming Wu
Keyword(s):  
Acrylic Acid ◽  
Freeze Drying ◽  
Crystallization Rate ◽  
X Ray Diffraction ◽  
Butylene Succinate ◽  
Covalent Bonds ◽  
Polymer Backbone ◽  
Transmission Electron ◽  
Degradation Rates ◽  
Organically Modified

Biodegradable acrylic acid-grafted poly(butylene succinate-co-terephthalate) (g-PBST)/organically modified layered zinc phenylphosphonate (m-PPZn) nanocomposites were effectively fabricated containing covalent bonds between the g-PBST and m-PPZn. The results of wide-angle X-ray diffraction and transmission electron microscopy revealed that the morphology of the g-PBST/m-PPZn nanocomposites contained a mixture of partially exfoliated or intercalated conformations. The isothermal crystallization behavior of the nanocomposites showed that the half-time for crystallization of 5 wt % g-PBST/m-PPZn nanocomposites was less than 1 wt % g-PBST/m-PPZn nanocomposites. This finding reveals that increasing the loading of m-PPZn can increase the crystallization rate of nanocomposites. Degradation tests of g-PBST/m-PPZn nanocomposites fabricated using the heat pressing and the freeze-drying process were performed by lipase from Pseudomonas sp. The degradation rates of g-PBST-50/m-PPZn nanocomposites were significantly lower than those of g-PBST-70/m-PPZn nanocomposites. The g-PBST-50 degraded more slowly due to the higher quantity of aromatic group and increased stiffness of the polymer backbone. The degradation rate of the freeze-drying specimens contained a more extremely porous conformation compared to those fabricated using the heat pressing process.

Reactive melt mixing of PC/PEN blend. Structural characterization of reaction products

Polymer ◽  
2015 ◽  
Vol 74 ◽  
pp. 108-123 ◽  
Author(s):  
Filippo Samperi ◽  
Salvatore Battiato ◽  
Giuseppe Recca ◽  
Concetto Puglisi ◽  
Raniero Mendichi
Keyword(s):  
Structural Characterization ◽  
Reaction Products ◽  
Melt Mixing ◽  
Reactive Melt

Chemical Exchange Reactions in Blends of the Biodegradable Polyester with poly(hydroxy ether of bisphenol-A)

2014 ◽  
Vol 953-954 ◽  
pp. 1246-1249 ◽  
Author(s):  
Chean Cheng Su ◽  
Chern Hwa Chen ◽  
Neng Lang Shih ◽  
Yin Shuo Li
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Differential Scanning Calorimetry ◽  
Bisphenol A ◽  
Chemical Exchange ◽  
Exchange Reactions ◽  
Scanning Calorimetry ◽  
Butylene Succinate ◽  
Butylene Terephthalate ◽  
Before And After ◽  
Hydroxy Ether

Compatibilization via transreactions in blends of poly (butylene succinate-co-butylene terephthalate) [P(BS-co-BT)] with poly (hydroxy ether of bisphenol-A) (phenoxy) were investigated. Analyses were based on characterization using differential scanning calorimetry (DSC) and solid-state nuclear magnetic resonance (NMR). They revealed that the P(BS-co-BT)/phenoxy blend had a phase morphology that could be homogenized only following annealing at high temperatures. As-blended P(BS-co-BT)/phenoxy (50/50 composition) exhibited immiscible phases with two distinct Tgs, but the initially phase separated blends finally merged to form a homogeneous phase with a single Tgupon heating and annealing for 60 min at 280 °C. Chemical exchange reactions upon heat-annealing were likely to have caused the phase homogenization in the P(BS-co-BT)/phenoxy blend. NMR was performed on blend samples before and after they were heated to 280 °C, but the similarity of bonds made obtaining straight results difficult. Results of this study demonstrate phase homogenization can be brought only upon heat-annealing in the P(BS-co-BT)/phenoxy blend.

Thermal and Thermomechanical Properties of Poly(butylene succinate) Nanocomposites

2008 ◽  
Vol 8 (4) ◽  
pp. 1679-1689 ◽  
Author(s):  
Mamookho E. Makhatha ◽  
Suprakas Sinha Ray ◽  
Joseph Hato ◽  
Adriaan S. Luyt
Keyword(s):  
Thermal Stability ◽  
Tensile Modulus ◽  
Melting Behavior ◽  
Mechanical Analysis ◽  
Thermomechanical Properties ◽  
Scanning Calorimetry ◽  
Melt Mixing ◽  
Butylene Succinate ◽  
Modulated Differential Scanning Calorimetry ◽  
Thermal Stability Of

This article describes the thermal and thermomechanical properties of poly(butylene succinate) (PBS) and its nanocomposites. PBS nanocomposites with three different weight ratios of organically modified synthetic fluorine mica (OMSFM) have been prepared by melt-mixing in a batch mixer at 140 °C. The structure and morphology of the nanocomposites were characterized by X-ray diffraction (XRD) analyses and transmission electron microscopy (TEM) observations that reveal the homogeneous dispersion of the intercalated silicate layers into the PBS matrix. The thermal properties of pure PBS and the nanocomposite samples were studied by both conventional and temperature modulated differential scanning calorimetry (DSC) analyses, which show multiple melting behavior of the PBS matrix. The investigation of the thermomechanical properties was performed by dynamic mechanical analysis. Results reveal significant improvement in the storage modulus of neat PBS upon addition of OMSFM. The tensile modulus of neat PBS is also increased substantially with the addition of OMSFM, however, the strength at yield and elongation at break of neat PBS systematically decreases with the loading of OMSFM. The thermal stability of the nanocomposites compared to that of the pure polymer sample was examined under both pyrolytic and thermooxidative environments. It is shown that the thermal stability of PBS is increased moderately in the presence of 3 wt% of OMSFM, but there is no significant effect on further silicate loading in the oxidative environment. In the nitrogen environment, however, the thermal stability systematically decreases with increasing clay loading.

Effects of reactive melt mixing on the morphology and thermal behavior of linear low-density polyethylene/rubber blends

2008 ◽  
Vol 109 (2) ◽  
pp. 1014-1021 ◽  
Author(s):  
Maurizio Penco ◽  
Stefania Della Sciucca ◽  
Elisa Passaglia ◽  
Guido Giordani ◽  
Serena Coiai ◽  
...  
Keyword(s):  
Thermal Behavior ◽  
Low Density Polyethylene ◽  
Low Density ◽  
Linear Low Density Polyethylene ◽  
Melt Mixing ◽  
Rubber Blends ◽  
Reactive Melt
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