Synthesis and properties of bismaleimide resins containing phthalide cardo and cyano groups

2018 ◽  
Vol 31 (4) ◽  
pp. 462-471 ◽  
Author(s):  
Siyang Liu ◽  
Yuanying Wang ◽  
Ping Chen ◽  
Dongwei Xu ◽  
Xuhai Xiong ◽  
...  
Keyword(s):  
Thermal Polymerization ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Carbon Fiber Composites ◽  
Scanning Calorimetry ◽  
Chemical Structures ◽  
Higher Temperature ◽  
Interlaminar Shear ◽  
Cyano Groups ◽  
Bismaleimide Resins

Two novel n ≈ 1 oligomeric bismaleimide monomers containing phthalide cardo and cyano groups (PCBMI and MCBMI) were designed and synthesized. The chemical structures of the monomers were confirmed from proton nuclear magnetic resonance spectroscopy and Fourier transform infrared spectroscopy. Both BMIs exhibit good solubility in common organic solvents, enabling easy solution processing. Thermal curing behaviors of the monomers were investigated by differential scanning calorimetry, displaying broad exothermic peaks and large thermal processing windows. Furthermore, PCBMI/carbon fiber composites were prepared, with their thermal stability and mechanical properties investigated. Thermogravimetric analysis and test of interlaminar shear strength indicated that the thermal polymerization of cyano groups improved the heat resistance of BMI resins and enhanced the interfacial adhesion at higher temperature.

scholarly journals Synthesis of Lactic Acid-Based Thermosetting Resins and Their Ageing and Biodegradability

Polymers ◽  
2020 ◽  
Vol 12 (12) ◽  
pp. 2849
Author(s):  
Lara Lopes Gomes Hastenreiter ◽  
Sunil Kumar Ramamoorthy ◽  
Rajiv K. Srivastava ◽  
Anilkumar Yadav ◽  
Akram Zamani ◽  
...  
Keyword(s):  
Lactic Acid ◽  
1H Nmr ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Soil Burial ◽  
Chemical Structures ◽  
Macro Scale ◽  
Ft Ir ◽  
Oxidative Ageing

The present work is focused on the synthesis of bio-based thermoset polymers and their thermo–oxidative ageing and biodegradability. Toward this aim, bio-based thermoset resins with different chemical architectures were synthesized from lactic acid by direct condensation with ethylene glycol, glycerol and pentaerythritol. The resulting branched molecules with chain lengths (n) of three were then end-functionalized with methacrylic anhydride. The chemical structures of the synthesized lactic acid derivatives were confirmed by proton nuclear magnetic resonance spectroscopy (1H-NMR) and Fourier transform infrared spectroscopy (FT–IR) before curing. To evaluate the effects of structure on their properties, the samples were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and the tensile testing. The samples went through thermo-oxidative ageing and biodegradation; and their effects were investigated. FT-IR and 1H-NMR results showed that three different bio-based resins were synthesized using polycondensation and end-functionalization. Lactic acid derivatives showed great potential to be used as matrixes in polymer composites. The glass transition temperature of the cured resins ranged between 44 and 52 °C. Pentaerythritol/lactic acid cured resin had the highest tensile modulus and it was the most thermally stable among all three resins. Degradative processes during ageing of the samples lead to the changes in chemical structures and the variations in Young’s modulus. Microscopic images showed the macro-scale surface degradation on a soil burial test.

Preparation and properties of shape-stabilized phase change material cellulose benzoate-g-polyoxyethylene (2) hexadecyl ether with potential for thermal energy storage

2018 ◽  
Vol 89 (8) ◽  
pp. 1512-1521
Author(s):  
Na Han ◽  
Wenxin Zhang ◽  
Xiufang Wang ◽  
Xingxiang Zhang ◽  
Wei Li ◽  
...  
Keyword(s):  
Phase Transition ◽  
Energy Storage ◽  
Phase Change ◽  
Thermal Energy ◽  
Thermal Energy Storage ◽  
Solid Phase ◽  
Resonance Spectroscopy ◽  
Thermal Reliability ◽  
Scanning Calorimetry ◽  
Chemical Structures

It is a worldwide challenge to efficiently use renewable resources to solve the current energy shortage. The existing cellulose-based material is incapable of proper power storage. In this study, a series of cellulose benzoate-g-polyoxyethylene (2) hexadecyl ether (CB-g-E2C16) solid–solid phase change materials were synthesized with cellulose as the skeleton and polyoxyethylene (2) hexadecyl ether (E2C16) as a functional side chain. The skeleton cellulose and benzoyl chloride restrict the free movement of the molecular chains of E2C16 above the phase transition temperature, leading to a solid–solid phase change. Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy were performed to investigate the chemical structures. The thermal energy-storage properties, thermal reliability and thermal stability of the CB-g-E2C16 were investigated by differential scanning calorimetry and thermogravimetry (TG) methods. The analysis results indicated that the E2C16 chains were successfully grafted onto the cellulose benzoate (CB) backbone and the copolymers exhibited typical solid–solid phase transition behavior. The enthalpy and degree of substitution of graft copolymers CB-g-E2C16 could be adjusted by changing the feeding ratio of the raw materials, reaction temperature and post-processing methods of CB. TG analysis results showed that the CB-g-E2C16 copolymers possessed good thermostability and they keep their stability up to 278℃. Compared with pure cellulose, CB-g-E2C16 copolymers could be dissolved in dimethyl sulfoxide and most of them could be dissolved in N, N-dimethylformamide.

scholarly journals Analysis of Bio-Based Fatty Esters PCM’s Thermal Properties and Investigation of Trends in Relation to Chemical Structures

2019 ◽  
Vol 9 (2) ◽  
pp. 225 ◽  
Author(s):  
Rebecca Ravotti ◽  
Oliver Fellmann ◽  
Nicolas Lardon ◽  
Ludger Fischer ◽  
Anastasia Stamatiou ◽  
...  
Keyword(s):  
Thermal Properties ◽  
Phase Change ◽  
Energy Demand ◽  
Phase Change Materials ◽  
Arachidic Acid ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Fatty Esters ◽  
Latent Heat Storage ◽  
Chemical Structures

As global energy demand increases while primary sources and fossil fuels’ availability decrease, research has shifted its focus to thermal energy storage systems as alternative technologies able to cover for the mismatch between demand and supply. Among the different phase change materials available, esters possess particularly favorable properties with reported high enthalpies of fusion, low corrosivity, low toxicity, low supercooling, thermal and chemical stability as well as biodegradability and being derived from renewable feedstock. Despite such advantages, little to no data on the thermal behavior of esters is available due to low commercial availability. This study constitutes a continuation of previous works from the authors on the investigation of fatty esters as novel phase change materials. Here, methyl, pentyl and decyl esters of arachidic acid, and pentyl esters of myristic, palmitic, stearic and behenic acid are synthesized through Fischer esterification with high purities and their properties are studied. The chemical structures and purities are confirmed through Attenuated Total Reflectance Infrared Spectroscopy, Gas Chromatography coupled with Mass Spectroscopy and Nuclear Magnetic Resonance Spectroscopy, while the determination of the thermal properties is performed through Differential Scanning Calorimetry and Thermogravimetric Analysis. In conclusion, some correlations between the melting temperatures and the chemical structures are discovered, and the fatty esters are assessed based on their suitability as phase change materials for latent heat storage applications.

scholarly journals Synthesis and Self-Assembly of Poly(N-Vinylcaprolactam)-b-Poly(ε-Caprolactone) Block Copolymers via the Combination of RAFT/MADIX and Ring-Opening Polymerizations

Polymers ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 1252
Author(s):  
Rodolfo M. Moraes ◽  
Layde T. Carvalho ◽  
Gizelda M. Alves ◽  
Simone F. Medeiros ◽  
Elodie Bourgeat-Lami ◽  
...  
Keyword(s):  
Block Copolymers ◽  
Ring Opening ◽  
Chain Transfer ◽  
Fluorescence Probe ◽  
Size Exclusion ◽  
Proton Nuclear Magnetic Resonance ◽  
Solution Temperature ◽  
Copolymer Composition ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry

Well-defined amphiphilic, biocompatible and partially biodegradable, thermo-responsive poly(N-vinylcaprolactam)-b-poly(ε-caprolactone) (PNVCL-b-PCL) block copolymers were synthesized by combining reversible addition-fragmentation chain transfer (RAFT) and ring-opening polymerizations (ROP). Poly(N-vinylcaprolactam) containing xanthate and hydroxyl end groups (X–PNVCL–OH) was first synthesized by RAFT/macromolecular design by the interchange of xanthates (RAFT/MADIX) polymerization of NVCL mediated by a chain transfer agent containing a hydroxyl function. The xanthate-end group was then removed from PNVCL by a radical-induced process. Finally, the hydroxyl end-capped PNVCL homopolymer was used as a macroinitiator in the ROP of ε-caprolactone (ε-CL) to obtain PNVCL-b-PCL block copolymers. These (co)polymers were characterized by Size Exclusion Chromatography (SEC), Fourier-Transform Infrared spectroscopy (FTIR), Proton Nuclear Magnetic Resonance spectroscopy (1H NMR), UV–vis and Differential Scanning Calorimetry (DSC) measurements. The critical micelle concentration (CMC) of the block copolymers in aqueous solution measured by the fluorescence probe technique decreased with increasing the length of the hydrophobic block. However, dynamic light scattering (DLS) demonstrated that the size of the micelles increased with increasing the proportion of hydrophobic segments. The morphology observed by cryo-TEM demonstrated that the micelles have a pointed-oval-shape. UV–vis and DLS analyses showed that these block copolymers have a temperature-responsive behavior with a lower critical solution temperature (LCST) that could be tuned by varying the block copolymer composition.

scholarly journals Synthesis and Characterization of Low-Cost Cresol-Based Benzoxazine Resins as Potential Binders in Abrasive Composites

Materials ◽  
2020 ◽  
Vol 13 (13) ◽  
pp. 2995
Author(s):  
Artur Jamrozik ◽  
Mateusz Barczewski ◽  
Grzegorz Framski ◽  
Daniel Baranowski ◽  
Paulina Jakubowska ◽  
...  
Keyword(s):  
Low Cost ◽  
2D Nmr ◽  
Additional Analysis ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Voc Emission ◽  
Chemical Structures ◽  
Oxazine Ring ◽  
Nmr Techniques

A series of cresol-based benzoxazines were synthesized for potential application as a polymer matrix in abrasive composites. The chemical structures of the obtained benzoxazine resins were investigated in detail using Fourier transform infrared spectroscopy (FTIR) and hydrogen-1 as well as carbon-13 nuclear magnetic resonance spectroscopy (1H NMR, 13C NMR) with an additional analysis using two-dimensional NMR techniques (2D NMR 1H-1H COSY, 1H-13C gHSQC and gHMBC). Structural analysis confirmed the presence of vibrations of -O-C-N- at ~950 cm−1 wavenumber, characteristic for an oxazine ring. The thermal properties of benzoxazine monomers were examined using differential scanning calorimetry (DSC) analysis. The polymerization enthalpy varied from 143.2 J/g to 287.8 J/g. Thermal stability of cresol-based benzoxazines was determined using thermogravimetry (TGA) analysis with additional analysis of the amount of volatile organic compounds (VOC) emitted from the synthesized benzoxazines during their crosslinking by static headspace coupled with gas chromatography technique (HS-GC). The amount of residual mass significantly differed between all synthesized polybenzoxazines in the range from 8.4% to 21.2%. The total VOC emission for benzoxazines decreased by 46–77% in reference to a conventional phenolic binder. The efficiency of abrasive composites with the benzoxazine matrix was evaluated based on abrasion tests. Performed analyses confirmed successful synthesis and proper chemical structure of cresol-based benzoxazines. All the experiments indicated that benzoxazines based on different cresol isomers significantly differ from each other. Good thermal performance and stability of the abrasive composites with the polybenzoxazine matrix and significantly lower VOC emission allow us to state that benzoxazines can be a promising and valuable alternative to the phenolics and a new path for the development of modern, eco-friendly abrasives.

Heat-resistant and photoluminescent indole-based poly(ether sulfone)s

2017 ◽  
Vol 30 (4) ◽  
pp. 475-479 ◽  
Author(s):  
Wenxuan Wei ◽  
Li Yang ◽  
Guanjun Chang
Keyword(s):  
Thermal Stability ◽  
High Performance ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Condensation Polymerization ◽  
High Glass Transition Temperature ◽  
Scanning Calorimetry ◽  
Good Thermal Stability ◽  
High Performance Polymers ◽  
Good Agreement

Indole-based poly(ether sulfone)s (PINESs), as novel high-performance polymers, have been obtained by the condensation polymerization of 4-hydroxyindole and hydroquinone with activated difluoro monomers via a catalyst-free nucleophilic substitution reaction. The structures of the polymers are characterized by means of Fourier transform infrared and proton nuclear magnetic resonance spectroscopy, and the results show good agreement with the proposed structures. Differential scanning calorimetry and thermogravimetric analysis measurements exhibit that polymers possess high glass transition temperature ( Tgs > 245°C) and good thermal stability with high decomposition temperatures ( Tds > 440°C). In addition, due to their special structure, PINESs are endowed with significantly strong photonic luminescence in N, N-dimethylformamide.

Chiral Liquid Crystal Polymers Containing Electron Donor- Acceptor Action-Synthesis and Characterization

2011 ◽  
Vol 284-286 ◽  
pp. 2284-2287
Author(s):  
Xiao Zhi He ◽  
Mei Tian ◽  
Yang Chen ◽  
Jing Zhao ◽  
Bao Yan Zhang
Keyword(s):  
Electron Donor ◽  
Liquid Crystalline ◽  
Proton Nuclear Magnetic Resonance ◽  
Liquid Crystal Polymers ◽  
Scanning Calorimetry ◽  
Cholesteric Phase ◽  
Chemical Structures ◽  
Heating And Cooling ◽  
Acceptor Group ◽  
Donor Acceptor

A series of new chiral side-chain liquid crystalline polymers with electron donor-acceptor action were prepared containing chiral monomer with donor group and nematic LC monomer with acceptor group. All polymers were synthesized by graft polymerization using polymethylhydro- siloxane as backbone. The mesomorphic properties were investigated by differential scanning calorimetry(DSC), polarizing optical microscopy(POM)，thermogravimetric analyses（TGA） and X-ray diffraction measurements(XRD). The chemical structures of monomers and polymers were confirmed by Fourier transform infrared (FTIR), proton nuclear magnetic resonance spectra(1H NMR and 13CNMR). M1 showed nematic phase and M2 turned out cholesteric phase on heating and cooling cycle. Polymers P3~P8 were cholesteric phase. Experimental results demonstrated that the glass transition temperatures and isotropization temperatures and the ranges of the mesophase temperature increased with increasing the content of chiral agent. All of the obtained polymers showed high thermal stability.

Thermal properties of a series of tetrafunctional fluorene-based oxazines/P-a blends

2016 ◽  
Vol 29 (10) ◽  
pp. 1139-1147 ◽  
Author(s):  
Zi Sang ◽  
Tiantian Feng ◽  
Wenbin Liu ◽  
Jun Wang ◽  
Mehdi Derradji
Keyword(s):  
Thermal Stability ◽  
Differential Scanning Calorimetry ◽  
Thermal Properties ◽  
Mechanical Analysis ◽  
Proton Nuclear Magnetic Resonance ◽  
Primary Amines ◽  
Resonance Spectroscopy ◽  
High Glass Transition Temperature ◽  
Scanning Calorimetry ◽  
Good Thermal Stability

A new series of aniline and aniline-mixed tetrafunctional fluorene-based oxazine monomers were synthesized using 2,7-hydroxy-9,9-bis-(4-hydroxyphenyl) fluorene, paraformaldehyde, and primary amines (including aniline or aniline mixed with n-butylamine or n-octylamine composition). Fourier transform infrared spectroscopy and proton nuclear magnetic resonance spectroscopy were used to characterize the structure of the monomers. The copolymers were obtained by adding the monomers into a typical monofunctional polybenzoxazine (phenol-aniline-based benzoxazine). Differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis were performed to study the thermal properties of the copolymers. The copolymers exhibited high glass transition temperature values (164–201°C). A good thermal stability was also obtained with a 5% weight loss temperature over 355°C and high char yields at 800°C (42–50%).

Synthesis and phase behavior of chiral liquid crystalline polymeric networks derived from menthol

2012 ◽  
Vol 24 (8) ◽  
pp. 673-682 ◽  
Author(s):  
Ying-Gang Jia ◽  
Jian-She Hu ◽  
Dan Li ◽  
Qing-Bao Meng ◽  
Xia Zhang
Keyword(s):  
Phase Behavior ◽  
Near Infrared ◽  
Polymer Networks ◽  
Crosslinking Agent ◽  
Proton Nuclear Magnetic Resonance ◽  
Scanning Calorimetry ◽  
Excellent Thermal Stability ◽  
Cholesteric Phase ◽  
Temperature Range ◽  
Chemical Structures

The synthesis of new chiral monomer 4-(menthyloxyacetoxy- benzoyloxy)biphenyl-4′-(2-(undec-10-e noyloxy)ethoxy)benzoate (ML), crosslinking agent 4-(undec-10-enoyloxy)biphenyl-4′-(2-(undec-10-enoyloxy)ethoxy)benzoate (CA), and liquid crystal polymer networks (E1−E5) containing menthyl group is presented. Their chemical structures and phase behavior were characterized with Fourier transform infrared (FT-IR), proton nuclear magnetic resonance (1H-NMR), elemental analyses, polarizing optical microscopy, differential scanning calorimetry, thermogravimetric analysis (TGA), and X-ray diffraction. The selective reflection of light for ML was investigated with ultraviolet/visible/near infrared (UV/Visible/NIR). By inserting a flexible spacer between the mesogenic core and the terminal menthyl groups, MLcould form mesophase and show a chiral smectic C phase, cholesteric phase and cubic blue phase. CA displayed a smectic A phase and nematic phase. The polymer networks containing less than 12 mol% of the crosslinking units showed reversible cholesteric phase transition, wide mesophase temperature range, and excellent thermal stability. With increasing the content of crosslinking unit, the corresponding Tg increased, the Ti decreased, and the mesophase temperature range narrowed for E1−E5. TGA showed that the Td(5%) was greater than 330°C for E1−E5.

scholarly journals Structural and Thermal Properties of Ethylene-Norbornene Copolymers Obtained Using Vanadium Homogeneous and SIL Catalysts

Polymers ◽  
2020 ◽  
Vol 12 (11) ◽  
pp. 2433
Author(s):  
Paweł Groch ◽  
Anna Bihun-Kisiel ◽  
Aleksandra Piontek ◽  
Wioletta Ochędzan-Siodłak
Keyword(s):  
Thermal Properties ◽  
Reactivity Ratio ◽  
Proton Nuclear Magnetic Resonance ◽  
Sequence Length ◽  
Resonance Spectroscopy ◽  
Scanning Calorimetry ◽  
Reaction Conditions ◽  
Copolymer Microstructure ◽  
Chain Termination Reaction ◽  
Catalyst Systems

The series of ethylene-norbornene (E-NB) copolymers was obtained using different vanadium homogeneous and supported ionic liquid (SIL) catalyst systems. The 13C and 1H NMR (carbon and proton nuclear magnetic resonance spectroscopy) together with differential scanning calorimetry (DSC) were applied to determine the composition of copolymers such as comonomer incorporation (CNB), monomer dispersity (MD), monomer reactivity ratio (re), sequence length of ethylene (le) and tetrad microblock distributions. The relation between the type of catalyst, reaction conditions and on the other hand, the copolymer microstructure, chain termination reaction analyzed by the type of unsaturation are discussed. In addition, the thermal properties of E-NB copolymers such as the melting and crystallization behavior, like also the heterogeneity of composition described by successive the self-nucleation and annealing (SSA) and the dispersity index (DI) were determined.

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