Synthesis and property studies of oligomer obtained from the reaction of 4-vinylbenzocyclobutene and styrene with divinyl tetramethyl disiloxane-bisbenzocyclobutene

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Yewei Xu ◽  
Fanghua Zhu ◽  
Liqin Xie ◽  
Junxiao Yang ◽  
Lin Zhang ◽  
...  
Keyword(s):  
Low Cost ◽  
Gel Permeation Chromatography ◽  
Radical Copolymerization ◽  
Film Material ◽  
Scanning Calorimetry ◽  
Cure Reaction ◽  
Good Thermal Stability ◽  
Molecular Weights ◽  
H Nmr ◽  
Polymer Resin

AbstractRadical copolymerization of 4-vinylbenzocyclobutene (VBCB) with styrene (St) afforded the copolymer (4-vinylbenzocyclobutene-co-styrene) (VBCBSt). Reaction of VBCB-St and divinyl tetramethyl disiloxane-bisbenzocyclobutene (DVSBCB) gave the oligomer (VBCB-St-DVSBCB), which was subsequently subjected to the cure reaction. The structures of VBCB-St and oligomer (VBCB-St- DVSBCB) were characterized by FTIR and 1H NMR, which are in agreement with the proposed structures. Molecular weights of the synthesized polymers were estimated by gel permeation chromatography (GPC). Differential scanning calorimetry (DSC) showed that VBCB-St exhibited glass transition temperature (Tg > 95 °C) however it is not the case for the oligomers (VBCB-St-DVSBCB). TG measurements indicated that the polymers had the good thermal stability with decomposition temperatures (TD > 370 °C). The polymer resin possessed good film planarization in the AFM images and the process of oligomer curing on a wafer without fusion and flow. These results indicated that the oligomer (VBCB-St- DVSBCB) is a promising film material with a relatively low cost.

Synthesis and Characterization of Poly (L-Lactic acid) Containing the Azobenzene Mesogens

2011 ◽  
Vol 181-182 ◽  
pp. 185-188
Author(s):  
Run Tao Dong ◽  
Qing Bin Xue ◽  
Ling Min Sun ◽  
Quan Xuan Zhang
Keyword(s):  
Lactic Acid ◽  
Optical Rotation ◽  
Gel Permeation Chromatography ◽  
Helical Structure ◽  
Feed Ratio ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
H Nmr ◽  
Azobenzene Mesogens

A series of azobenzene containing group Poly (L-lactic acid) (PLLA) were synthesized by Ring-Opening Polymerization of L-lactide (L-LA) catalysted by Sn (Oct)2initiated by alcohol-OH containing the azobenzene chromophores. Their molecular weights were well controlled by the feed ratio as characterized by Gel Permeation Chromatography (GPC) and1H NMR Spectrometry and agreed well with theoretical values. The thermal properties and liquid crystal phases were investigated by Differential Scanning Calorimetry (DSC), polarized optical microscopy (POM) and X-ray Diffraction (XRS) measurements. Cis-trans photoisomerization behavior of the polymers in the solutions and the films were studied with UV irradiation. By the Circular Dichroism Spectroscopy (CD) characterization of the solutions and films of the polymer, the PLLA segments show huge optical rotation power in helical structure.

“Nascent” Fe(0)-mediated living radical copolymerization of styrene and acrylonitrile

e-Polymers ◽  
2014 ◽  
Vol 14 (3) ◽  
pp. 187-192
Author(s):  
Guo-Xiang Wang ◽  
Mang Lu ◽  
Zhao-Hui Hou ◽  
Xue-Hui Zhan ◽  
Yong Gao ◽  
...  
Keyword(s):  
Gel Permeation Chromatography ◽  
Random Copolymer ◽  
Monomer Conversion ◽  
Radical Copolymerization ◽  
Chain Extension ◽  
Molar Ratio ◽  
Molecular Weights ◽  
H Nmr ◽  
First Order Kinetics

AbstractIn this work, we reported the synthesis of copolymers of poly(styrene-co-acrylonitrile) via single-electron transfer-living radical polymerization using CCl4 as an initiator and Zn(0)/2,2′-bipyridine (Bpy)/FeCl2 as catalyst complexes. The polymerization was carried out at 25°C. The polymerization proceeded in a living fashion based on “nascent” Fe(0) as the source of the transition metal, which was prepared by Zn(0)/FeCl2 in situ. The kinetic experimental results showed that the copolymerization is first-order kinetics. The molecular weights increased linearly with respect to monomer conversion, and narrow polydispersity index values were obtained. The effect of the molar ratio of [Zn(0)]0/[FeCl2]0 on polymerization was investigated. In addition, the polymerization carried out in different solvents was also investigated. The obtained random copolymer was characterized by 1H NMR and gel permeation chromatography. The living characteristic was demonstrated by chain extension experiment.

Characterization of bi-layered magnetic nanoparticles synthesized via two-step surface-initiated ring-opening polymerization

2015 ◽  
Vol 87 (11-12) ◽  
pp. 1085-1097 ◽  
Author(s):  
Li Wang ◽  
Stefan Baudis ◽  
Karl Kratz ◽  
Andreas Lendlein
Keyword(s):  
Magnetic Nanoparticles ◽  
Ring Opening ◽  
Average Molecular Weight ◽  
Polymer Networks ◽  
Gel Permeation Chromatography ◽  
Degree Of Crystallinity ◽  
Scanning Calorimetry ◽  
H Nmr ◽  
Transmission Electron

AbstractA versatile strategy to integrate multiple functions in a polymer based material is the formation of polymer networks with defined nanostructures. Here, we present synthesis and comprehensive characterization of covalently surface functionalized magnetic nanoparticles (MNPs) comprising a bi-layer oligomeric shell, using Sn(Oct)2 as catalyst for a two-step functionalization. These hydroxy-terminated precursors for degradable magneto- and thermo-sensitive polymer networks were prepared via two subsequent surface-initiated ring-opening polymerizations (ROPs) with ω-pentadecalactone and ε-caprolactone. A two-step mass loss obtained in thermogravimetric analysis and two distinct melting transitions around 50 and 85°C observed in differential scanning calorimetry experiments, which are attributed to the melting of OPDL and OCL crystallites, confirmed a successful preparation of the modified MNPs. The oligomeric coating of the nanoparticles could be visualized by transmission electron microscopy. The investigation of degrafted oligomeric coatings by gel permeation chromatography and 1H-NMR spectroscopy showed an increase in number average molecular weight as well as the presence of signals related to both of oligo(ω-pentadecalactone) (OPDL) and oligo(ε-caprolactone) (OCL) after the second ROP. A more detailed analysis of the NMR results revealed that only a few ω-pentadecalactone repeating units are present in the degrafted oligomeric bi-layers, whereby a considerable degree of transesterification could be observed when OPDL was polymerized in the 2nd ROP step. These findings are supported by a low degree of crystallinity for OPDL in the degrafted oligomeric bi-layers obtained in wide angle X-ray scattering experiments. Based on these findings it can be concluded that Sn(Oct)2 was suitable as catalyst for the preparation of nanosized bi-layered coated MNP precursors by a two-step ROP.

Synthesis and characterization of novel methacrylate copolymers having pendant piperonyl group: monomer reactivity ratio, thermal degradation kinetics, and biological activity

2021 ◽  
Vol 29 (9_suppl) ◽  
pp. S1432-S1445
Author(s):  
Ibrahim Erol ◽  
Bayram Gencer ◽  
Zeki Gurler
Keyword(s):  
Biological Activity ◽  
Degradation Kinetics ◽  
Gel Permeation Chromatography ◽  
Reactivity Ratio ◽  
Thermal Degradation Kinetics ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
Monomer Reactivity Ratio ◽  
Bacteria And Fungi ◽  
Photo Stability

In this study, 2-{[(2H-1,3-benzodioxol-5-yl)methyl]amino}-2-oxoethyl 2-methylprop-2-enoate (BMAOME) monomer was synthesized, and copolymers were prepared with glycidyl methacrylate (GMA). Structural characterizations of the compounds were performed using FTIR, 1H-, and 13C-NMR techniques. Monomer reactivity ratio values were calculated by Finemann–Ross (FR) and Kelen–Tudos (KT) methods. The Tg value of the polymers was determined by differential scanning calorimetry (DSC) and their thermal stability was determined by thermogravimetric analysis (TGA). The molecular weights (w and n) and polydispersity index of the polymers were determined by gel permeation chromatography. The Ea value of thermal decomposition was determined by using the Ozawa and Kissinger methods. The photo-stability of the copolymers was investigated. Furthermore, the photo-stability of the copolymers and the biological activity of polymers against different types of bacteria and fungi were investigated.

Consequence of cenosphere loading on hygrothermal, thermal, and mechanical properties of epoxy syntactic foams

2019 ◽  
Vol 55 (3) ◽  
pp. 297-318 ◽  
Author(s):  
Mandip Kaur ◽  
LS Jayakumari
Keyword(s):  
Neat Epoxy ◽  
Homogeneous Distribution ◽  
Syntactic Foams ◽  
Scanning Calorimetry ◽  
Electron Microscopic ◽  
Cure Reaction ◽  
Good Thermal Stability ◽  
Specific Strength ◽  
Specific Modulus ◽  
Scanning Electron

Epoxy syntactic foams with different compositions of cenosphere were fabricated and characterised. The effect of loading cenosphere in epoxy syntactic foams was analysed. Good thermal stability of cenosphere–epoxy syntactic foams was established from the thermogravimetric analysis results. The completion of cure reaction at ambient temperature conditions was ascertained from differential scanning calorimetry results. Dynamic mechanical analysis revealed 114°C as the glass transition temperatures ( Tg) for neat epoxy sample, which increased to 132°C with 50% loading of cenosphere. Cenosphere-filled epoxy syntactic foams had low density and low water absorption values when compared to the neat epoxy sample. Homogeneous distribution of the cenosphere particles was confirmed using scanning electron microscopy. The compression studies confirmed brittle failure of the syntactic foams. This was also supported by the scanning electron microscopic images. The incorporation of hollow cenosphere particles led to a decrease in the flexural strength. Syntactic foams with 30% loading of cenosphere exhibited best specific modulus and specific strength. The specific strength increased by 24% for T30 sample and specific modulus increased by 36% for T30 samples when compared to the neat epoxy sample. As the need for strong but lightweight thermally stable products is continually increasing, there is a great possibility for the utilisation of these cenosphere–epoxy syntactic foams as lightweight core for sandwich composites.

scholarly journals Methylene-Bridged Tridentate Salicylaldiminato Binuclear Titanium Complexes as Copolymerization Catalysts for the Preparation of LLDPE through [Fe]/[Ti] Tandem Catalysis

Polymers ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 1114 ◽  
Author(s):  
Yani Luo ◽  
Jian Li ◽  
Derong Luo ◽  
Qingliang You ◽  
Zifeng Yang ◽  
...  
Keyword(s):  
Molecular Weight ◽  
High Temperature ◽  
Gel Permeation Chromatography ◽  
13C Nmr Spectroscopy ◽  
Molar Ratio ◽  
Tandem Catalysis ◽  
Titanium Complexes ◽  
Scanning Calorimetry ◽  
Molecular Weights ◽  
Branching Degree

A novel tandem catalysis system consisted of salicylaldiminato binuclear/mononuclear titanium and 2,6-bis(imino)pyridyl iron complexes was developed to catalyze ethylene in-situ copolymerization. Linear low-density polyethylene (LLDPE) with varying molecular weight and branching degree was successfully prepared with ethylene as the sole monomer feed. The polymerization conditions, including the reaction temperature, the Fi/Ti molar ratio, and the structures of bi- or mononuclear Ti complexes were found to greatly influence the catalytic performances and the properties of obtained polymers. The polymers were characterized by differential scanning calorimetry (DSC), high temperature gel permeation chromatography (GPC) and high temperature 13C NMR spectroscopy, and found to contain ethyl, butyl, as well as some longer branches. The binuclear titanium complexes demonstrated excellent catalytic activity (up to 8.95 × 106 g/molTi·h·atm) and showed a strong positive comonomer effect when combined with the bisiminopyridyl Fe complex. The branching degree can be tuned from 2.53 to 22.89/1000C by changing the reaction conditions or using different copolymerization pre-catalysts. The melting points, crystallinity and molecular weights of the products can also be modified accordingly. The binuclear complex Ti2L1 with methylthio sidearm showed higher capability for comonomer incorporation and produced polymers with higher branching degree and much higher molecular weight compared with the mononuclear analogue.

scholarly journals Lipase mediated synthesis of polycaprolactone and its silica nanohybrid

2019 ◽  
Vol 91 (6) ◽  
pp. 957-965
Author(s):  
Meltem Akkulak ◽  
Yasemin Kaptan ◽  
Yasar Andelib Aydin ◽  
Yuksel Avcibasi Guvenilir
Keyword(s):  
Average Molecular Weight ◽  
Proton Nuclear Magnetic Resonance ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Structural Investigations ◽  
Crystallinity Degree ◽  
Molecular Weights ◽  
H Nmr

Abstract In this study, rice husk ash (RHA) silanized with 3-glycidyloxypropyl trimethoxysilane was used as support material to immobilize Candida antarctica lipase B. The developed biocatalyst was then utilized in the ring opening polymerization (ROP) of ε-caprolactone and in situ development of PCL/Silica nanohybrid. The silanization degree of RHA was determined as 4 % (w) by thermal gravimetric analysis (TGA). Structural investigations and calculation of molecular weights of nanohybrids were realized by proton nuclear magnetic resonance (1H NMR). Crystallinity was determined by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Scanning Electron Microscopy (SEM) was used for morphological observations. Accordingly, the PCL composition in the nanohybrid was determined as 4 %, approximately. Short chained amorphous PCL was synthesized with a number average molecular weight of 4400 g/mol and crystallinity degree of 23 %. In regards to these properties, synthesized PCL/RHA composite can find use biomedical applications.

Novel bio-based epoxidized cardanol/cenosphere syntactic foams

2016 ◽  
Vol 29 (7) ◽  
pp. 785-796 ◽  
Author(s):  
Mandip Kaur ◽  
LS Jayakumari
Keyword(s):  
Sea Water ◽  
Homogeneous Distribution ◽  
Syntactic Foams ◽  
Scanning Calorimetry ◽  
Electron Microscopic ◽  
Sem Images ◽  
Fresh Sample ◽  
Cure Reaction ◽  
Casting Technique ◽  
Good Thermal Stability

Cenosphere-filled epoxidized cardanol syntactic foams were fabricated using stir-casting technique: 10–40 wt% of cenosphere was mixed gradually in several steps in order to avoid any damage of the cenosphere. The syntactic foams were cured at room temperature for a day followed by postcure for 3 h at 100°C. Completion of the cure reaction was ascertained using differential scanning calorimetry of the fresh sample and postcured sample. Homogeneous distribution of cenosphere was confirmed with the scanning electron microscopic (SEM) images. The fracture mechanism was also analysed using SEM image of the compression failed sample. Thermal, hygrothermal and compressive properties of the syntactic foams were studied. Epoxidized cardanol-based syntactic foams were found to have lower density, good thermal stability and higher char residue as revealed from the thermogravimetric analysis result. The yield strength decreased with the increase in cenosphere. The specific modulus was optimum for 30% loading of cenosphere and it increased by 42% in comparison to the neat sample. Hygrothermal studies conducted using deionized water and sea water at room and high temperature conditions revealed stability and lower water absorption. The bio-based syntactic foams derived from cardanol promised sustainable path for the preparation of light-weight foam core materials.

Cationic copolymerization of 1,3-pentadiene with α-pinene

2014 ◽  
Vol 34 (7) ◽  
pp. 583-589 ◽  
Author(s):  
Ai-Yuan Li ◽  
Xiang-Dong Sun ◽  
Hui-Bo Zhang ◽  
Yong-Chun Zhang ◽  
Bin Wang ◽  
...  
Keyword(s):  
Average Molecular Weight ◽  
Gel Permeation Chromatography ◽  
Polymerization Temperature ◽  
Scanning Calorimetry ◽  
Gardner Color ◽  
H Nmr ◽  
Cationic Copolymerization ◽  
Ft Ir ◽  
Better Than ◽  
C Nmr

Abstract The cationic copolymerization of 1,3-pentadiene (PD) with α-pinene (AP) initiated by aluminum trichloride (AlCl3) was carried out in N-pentane solvent. The effects of the polymerization temperature and the comonomer composition on the yield of the copolymer, softening point, Gardner color scale and number-average molecular weight (Mn) are discussed. The performance of the copolymer was better than that of AP homopolymer (PAP) and PD homopolymer (PPD). The structure of the copolymer was characterized by Fourier transform infrared spectroscopy (FT-IR), 1H-nuclear magnetic resonance (1H-NMR), 13C-NMR, differential scanning calorimetry (DSC) and gel permeation chromatography (GPC). In addition, the reactivity ratios for AP (M1) and PD (M2) determined by the Kelen-Tudos method from low-conversion data are r1=0.58 and r2=5.92, respectively.

Synthesis and Characterization of Linear Polymers for Non-Linear Optics through Click Chemistry Route

2012 ◽  
Vol 584 ◽  
pp. 8-12 ◽  
Author(s):  
Balakrishna Kolli ◽  
Sarada P. Mishra ◽  
Mukesh P. Joshi ◽  
S. Raj Mohan ◽  
T.S. Dhami ◽  
...  
Keyword(s):  
Click Chemistry ◽  
Second Harmonic ◽  
Gel Permeation Chromatography ◽  
Linear Polymers ◽  
Linear Optics ◽  
Scanning Calorimetry ◽  
Force Microscopy ◽  
Molecular Weights ◽  
Non Linear Optics ◽  
Atomic Force

Click chemistry is used for synthesizing polymers for second order NLO study. The molecular weights found by gel-permeation chromatography (GPC), were in the range of 7000-55000 g/mol. Differential scanning calorimetry shows glass transition temperature (Tg) above 120 oC. From electronic spectra order parameter of the poled films were calculated to be 0.1-0.5. The change in surface morphology after poling was checked by atomic force microscopy. By using a pulsed Nd:YAG laser (1064nm), the second harmonic generation (SHG) intensity was measured. The SHG intensity was also studied as a function of against temperature and time respectively.

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