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Synthesis and Characterization of Block Copolymers of Poly(silylene diethynylbenzen) and Poly(silylene dipropargyl aryl ether).

ABSTRACT: Poly(silylene diethynylbenzene)-b-poly(silylene dipropargyloxy diphenyl propane) copolymer (ABA-A), poly(silylene diethynylbenzene)-b-poly(silylene dipropargyloxy diphenyl ether) copolymer (ABA-O), and a contrast poly(silylene diethynylbenzene) with equivalent polymerization degree were synthesized through Grignard reactions. The structures and properties of the copolymers were investigated via hydrogen nuclear magnetic resonance, Fourier transform infrared spectroscopy, Haake torque rheometer, differential scanning calorimetry, dynamic mechanical analysis, thermogravimetric analysis and mechanical tests. The results show that the block copolymers possess comprehensive properties, especially good processability and good mechanical properties. The processing windows of these copolymers are wider than 58 °C. The flexural strength of the cured ABA-A copolymer reaches as high as 40.2 MPa. The degradation temperatures at 5% weight loss (T_d5) of the cured copolymers in nitrogen are all above 560 °C.

SUBMITTER: Gao M

PROVIDER: S-EPMC8125851 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Precise Synthesis and Thermoresponsive Property of Poly(ethyl glycidyl ether) and Its Block and Statistic Copolymers with Poly(glycidol).

Project description:In this paper, we describe a comprehensive study of the thermoresponsive properties of statistic copolymers and multiblock copolymers synthesized by poly(glycidol)s (PG) and poly(ethyl glycidyl ether) (PEGE) with different copolymerization methods. These copolymers were first synthesized by ring-opening polymerization (ROP), which was initiated by tert-butylbenzyl alcohol (tBBA) and 1-tert-butyl-4,4,4-tris(dimethylamino)-2,2-bis[tris(dimethylamino)phosphoranylidenamino]-2Λ5,4Λ5-catenadi(phosphazene) (t-Bu-P4) as the catalyst, and then the inherent protective groups were removed to obtain the copolymers without any specific chain end groups. The thermoresponsive property of the statistic copolymer PGx-stat-PEGEy was compared with the diblock copolymer PGx-b-PEGEy, and the triblock copolymers were compared with the pentablock copolymers. Among them, PG-stat-PEGE, PG-b-PEGE-b-PG-b-PEGE-b-PG, and PEGE-b-PG-b-PEGE-b-PG-b-PEGE, and even the specific ratio of PEGE-b-PG-b-PEGE, exhibited LCST-type phase transitions in water, which were characterized by cloud point (Tcp). Although the ratio of x to y affected the value of the Tcp of PGx-stat-PEGEy, we found that the disorder of the copolymer has a decisive effect on the phase-transition behavior. The phase-transition behaviors of PG-b-PEGE, part of PEGE-b-PG-b-PEGE, and PG-b-PEGE-b-PG copolymers in water present a two-stage phase transition, that is, firstly LCST-type and then the upper critical solution temperature (UCST)-like phase transition. In addition, we have extended the research on the thermoresponsive properties of EGE homopolymers without specific α-chain ends.

| S-EPMC8623496 | biostudies-literature

Tannic Acid-Mediated Aggregate Stabilization of Poly(N-vinylpyrrolidone)-b-poly(oligo (ethylene glycol) methyl ether methacrylate) Double Hydrophilic Block Copolymers.

Project description:The self-assembly of block copolymers in aqueous solution is an important field in modern polymer science that has been extended to double hydrophilic block copolymers (DHBC) in recent years. In here, a significant improvement of the self-assembly process of DHBC in aqueous solution by utilizing a linear-brush macromolecular architecture is presented. The improved self-assembly behavior of poly(N-vinylpyrrolidone)-b-poly(oligo(ethylene glycol) methyl ether methacrylate) (PVP-b-P(OEGMA)) and its concentration dependency is investigated via dynamic light scattering (DLS) (apparent hydrodynamic radii ? 100-120 nm). Moreover, the DHBC assemblies can be non-covalently crosslinked with tannic acid via hydrogen bonding, which leads to the formation of small aggregates as well (apparent hydrodynamic radius ? 15 nm). Non-covalent crosslinking improves the self-assembly and stabilizes the aggregates upon dilution, reducing the concentration dependency of aggregate self-assembly. Additionally, the non-covalent aggregates can be disassembled in basic media. The presence of aggregates was studied via cryogenic scanning electron microscopy (cryo-SEM) and DLS before and after non-covalent crosslinking. Furthermore, analytical ultracentrifugation of the formed aggregate structures was performed, clearly showing the existence of polymer assemblies, particularly after non-covalent crosslinking. In summary, we report on the completely hydrophilic self-assembled structures in solution formed from fully biocompatible building entities in water.

| S-EPMC6566864 | biostudies-literature

1,4-D-Glucan block copolymers: synthesis and comprehensive structural characterization.

Project description:Multi-block glucans comprising permethylated and partially methylated blocks are compounds of interest. In order to monitor their formation by transglycosylation of corresponding starting glucans, a method has been developed and applied to model compounds. This method allows determining the average length of the blocks and the progress of incorporation of methyl blocks in partially methylated sequences with a random distribution. The method, comprising liquid chromatography mass spectrometry (LC-MS) and electrospray ionization collision-induced dissociation tandem mass spectrometry (ESI-CID-MSn) measurements of two types of peralkylated glucans representing derivatives of the target compounds, is comprehensively described and discussed. ESI-MSn allows looking into the sequences of oligomeric domains. In addition, transglycosylation is followed by attenuated total reflection FTIR and NMR spectroscopy. Graphical abstract.

| S-EPMC7026270 | biostudies-literature

Synthesis and Characterization of N-Substituted Polyether-Block-Amide Copolymers.

Project description:A series of N-substituted polyether-block-amide (PEBA-X%) copolymers were prepared by melt polycondensation of nylon-6 prepolymer and polytetramethylene ether glycol at an elevated temperature using titanium isopropoxide as a catalyst. The structure, thermal properties, and crystallinity of PEBA-X% were investigated using nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectroscopy, differential scanning calorimetry, wide angle X-ray diffraction, and thermogravimetric analysis. In general, the crystallinity, melting point, and thermal degradation temperature of PEBA-X% decreased as the incorporation of N-methyl functionalized groups increased, owing to the disruption caused to the structural regularity of the copolymer. However, in N-acetyl functionalized analogues, the crystallinity first dropped and then increased because of a new γ form arrangement that developed in the microstructure. After the cross-linking reaction of the N-methyl-substituted derivative, which has electron-donating characteristics, with poly(4,4'-methylenebis(phenyl isocyanate), the decomposition temperature of the resulting polymer significantly increased, whereas no such improvements could be observed in the case of the electro-withdrawing N-acetyl-substituted derivative, because of the incompleteness of its cross-linking reaction.

| S-EPMC7915099 | biostudies-literature

Synthesis and Characterization of Phosphorus- and Carborane-Containing Polyoxanorbornene Block Copolymers.

Project description:Grubbs-catalyzed ring-opening metathesis polymerization (ROMP) of carborane- and phosphonate-containing monomers has been used for the generation of hybrid block copolymers. Molecular weights with Mn of 50,000 g/mol were readily obtained with polydispersity index values, ?, between 1.03?1.08. Reaction of the phospha ester and carborane substituted oxanorbornene block copolymer with trimethylsilyl bromide led to a new polymer with phosphonic acid functionalities. In application studies, the phospha-carborane functionalized block polymer was tested as heat resistance material. Thermal stability was investigated by thermal gravimetric analysis (TGA) and microscale combustion calorimetry (MCC) analysis. Thermal treatment and ceramic yield under air were directly correlated to the carborane content of the block copolymer. However, phosphorus content in the polymer was more crucial for the char residues when heated under nitrogen atmosphere. The peak heat release rate (PHRR) increased as the number of phosphonate functionalities increased. However, corresponding phosphonic acid derivatives featured a lower heat release rate and total heat release. Moreover, the phosphonic acid functionalities of the block copolymer offer efficient chelating capabilities for iron nanoparticles, which is of interest for applications in biomedicine in the future. The complexation with iron oxide nanoparticles was studied by transmission electron microscopy (TEM) and inductively coupled plasma mass spectrometry (ICP?MS).

| S-EPMC6523416 | biostudies-literature

Cell Engineering with Functional Poly(oxanorbornene) Block Copolymers.

Project description:Cell-based therapies are gaining prominence in treating a wide variety of diseases and using synthetic polymers to manipulate these cells provides an opportunity to impart function that could not be achieved using solely genetic means. Herein, we describe the utility of functional block copolymers synthesized by ring-opening metathesis polymerization (ROMP) that can insert directly into the cell membrane via the incorporation of long alkyl chains into a short polymer block leading to non-covalent, hydrophobic interactions with the lipid bilayer. Furthermore, we demonstrate that these polymers can be imbued with advanced functionalities. A photosensitizer was incorporated into these polymers to enable spatially controlled cell death by the localized generation of 1 O2 at the cell surface in response to red-light irradiation. In a broader context, we believe our polymer insertion strategy could be used as a general methodology to impart functionality onto cell-surfaces.

| S-EPMC7482174 | biostudies-literature

Synthesis of Di-Block Copolymers Poly (propylene ox-ide)-block-Poly (9-(2,3-epoxypropyl) Carbazole) via Sequential Addition of Monomers in One Pot.

Project description:Polypropylene oxide (PPO) and poly(9-(2,3-epoxypropyl) carbazole) (PEPK) di-block copolymers are prepared in one pot via sequential monomer addition by using i-PrONa/i-Bu3Al as an anionic catalytic system. An almost 100% monomer conversion is obtained, and the length of each block is controlled through the monomer/catalyst ratio used. Copolymer molecular weights are quite close to theoretical values calculated assuming the formation of one polymer chain per catalyst; therefore, it is hypothesized that the polymerization reaction proceeds with a living character. The synthesis appears to be particularly efficient and versatile. The calorimetric properties of copolymers obtained in this work are remarkable, since they show two distinct Tg values, corresponding to the PPO and PEPK blocks. The optical measurements of di-block copolymers show more analogous features than those of PEPK homopolymer. Copolymer solution emission spectra just exhibit isolated carbazole fluorescence, whereas in the solid state, film spectra show excimer fluorescence.

| S-EPMC7957571 | biostudies-literature

Synthesis of a Regioregular Series of Poly(aryl ether carbonates) and Their Glass Transition Temperatures.

Project description:Bisphenol A polycarbonate (BPA-PC) is a remarkable high-performance engineering polymer, although it is susceptible to photo-Fries and hydrolytic degradation. New poly(aryl ether carbonates) were synthesized to address these limitations by replacing the chain backbone carbonate ester functionality with aryl ether functionality. The monomers for these new polymers were synthesized by a variation of the Ullmann condensation accelerated by 2,2,6,6-tetramethylheptane-3,5-dione and promoted by Cs2CO3 and 1-methyl-2-pyrrolidinone under mild conditions. Four such bisphenol A-based diarylether monomers containing different mass ratios of carbonate ester groups were prepared and polymerized with phosgene gas to give novel poly(aryl ether carbonates). Polymers were named as di-o-BPA-PC 9', tri-o-BPA-PC 11', tetra-o-BPA-PC 13', and penta-o-BPA-PC 15' where di-, tri-, tetra-, and penta- reflect the number of diphenylisopropylidene units in each of the respective polymers. The molecular weights of the resulting four poly(aryl ether carbonates) were measured by gel permeation chromatography. Differential scanning calorimetry was used to measure glass transition temperature (T g). The polymers exhibited weight-average molecular weights up to 4.09 × 105 g/mol and T g in the range of 136 to 149 °C with no melting temperature peak, indicative of their amorphous character. The new polymers formed transparent and flexible films by solution casting from chloroform solution.

| S-EPMC6941183 | biostudies-literature

Synthesis, Properties, and Enzymatic Hydrolysis of Poly(lactic acid)-co-Poly(propylene adipate) Block Copolymers Prepared by Reactive Extrusion.

Project description:Poly(lactic acid) (PLA) is a biobased polyester with ever-growing applications in the fields of packaging and medicine. Despite its popularity, it suffers from inherent brittleness, a very slow degradation rate and a high production cost. To tune the properties of PLA, block copolymers with poly(propylene adipate) (PPAd) prepolymer were prepared by polymerizing L-lactide and PPAd oligomers via reactive extrusion (REX) in a torque rheometer. The effect of reaction temperature and composition on the molecular weight, chemical structure, and physicochemical properties of the copolymers was studied. The introduction of PPAd successfully increased the elongation and the biodegradation rate of PLA. REX is an efficient and economical alternative method for the fast and continuous synthesis of PLA-based copolymers with tunable properties.

| S-EPMC8659515 | biostudies-literature

Nanocomposite Based on Functionalized Gold Nanoparticles and Sulfonated Poly(ether ether ketone) Membranes: Synthesis and Characterization.

Project description:Gold nanoparticles, capped by 3-mercapto propane sulfonate (Au-3MPS), were synthesized inside a swollen sulfonated poly(ether ether ketone) membrane (sPEEK). The formation of the Au-3MPS nanoparticles in the swollen sPEEK membrane was observed by spectroscopic and microscopic techniques. The nanocomposite containing the gold nanoparticles grown in the sPEEK membrane, showed the plasmon resonance λmax at about 520 nm, which remained stable over a testing period of three months. The size distribution of the nanoparticles was assessed, and the sPEEK membrane roughness, both before and after the synthesis of nanoparticles, was studied by AFM. The XPS measurements confirm Au-3MPS formation in the sPEEK membrane. Moreover, AFM experiments recorded in fluid allowed the production of images of the Au-3MPS@sPEEK composite in water at different pH levels, achieving a better understanding of the membrane behavior in a water environment; the dynamic hydration process of the Au-3MPS@sPEEK membrane was investigated. These preliminary results suggest that the newly developed nanocomposite membranes could be promising materials for fuel cell applications.

| S-EPMC5503356 | biostudies-literature

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