Synthesis and properties of (A2+B4)-type hyperbranched polyimides with different terminal groups

2016 ◽  
Vol 29 (1) ◽  
pp. 46-57 ◽  
Author(s):  
Shanyou Liu ◽  
Shiyang Zhu ◽  
Xueping Wang ◽  
Haiwei Tan ◽  
Shaowei Guan

To investigate the effect of terminal groups on the properties of hyperbranched polyimides (HBPIs) for potential optical applications, a series of HBPIs bearing different terminal groups have been synthesized through a novel aromatic CF3-containing tetra-amine, 4,4′-di[3,5-di(2-trifluoromethyl-4-aminophenoxy)phenoxy] sulfone, and a long chain dianhydride, 2,2-bis[4-(3,4-dicarboxyphenoxy)phenyl]hexafluoropropane, via a two-step polycondensation procedure. The synthesized HBPIs could form flexible and tough polyimide (PI) films, which exhibit good thermal stability with the glass transition temperatures of 191–234°C for differential scanning calorimetry measurement, the 5% weight loss temperatures of 533–610°C, and residual weights of 45.8–58.6% at 800°C under nitrogen atmosphere. The PI films have favorable mechanical properties with tensile strengths of 77–92 MPa, elongation at break of 3.55–7.99%, and initial modulus of 2.05–2.86 GPa. The films also exhibit the good transmittance of higher than 80% at 800 nm. The average refractive indices ( nav) and in-plane/out-of-plane birefringence (Δ n) measured at 632.8 nm are in the range of 1.5539–1.6022 and 0.0065–0.0077, respectively. The good transmittance in the visible region, tunable nav, and low Δ n are very suitable for optical applications.

2008 ◽  
Vol 37 (1) ◽  
pp. 21-27
Author(s):  
H. Satapathy ◽  
A.K. Banthia

PurposeThe purpose of this paper is to synthesise, characterise and study polymerisation kinetics of novel 4‐nonylphenylmethacrylate (NPMA) polymer.Design/methodology/approachNew methacrylic monomer, 4‐NPMA with a pendant nonylphenyl group was synthesised and characterised using various characterisation techniques. The free radical polymerisation kinetics study was done with the help of differential scanning calorimetry data.FindingsThe average heat of polymerisation (ΔHp) was found to be 685.43 J/g. Activation energy (Ea) of 95.86 kJ mol−1 and frequency factor of (A) 3.4 × 104 min−1 was obtained using Kissinger method. The thermogravimetric analysis of the polymer in nitrogen reveals that it possesses very good thermal stability in comparison to alkyl methacrylates due to presence of pendant nonylphenyl group.Research limitations/implicationsNew methacrylic monomer, 4‐NPMA was synthesised by reacting nonylphenol dissolved in methyl ethyl ketone (MEK) with methacryloyl chloride in the presence of triethylamine as a base. Polymerisation of 4‐NPMA was carried out in MEK using benzoyl peroxide (BPO) as initiator under nitrogen atmosphere. The kinetics study of NPMA monomer with 1.1 wt% BPO was reported for evaluation of kinetic parameters by employing the Kissinger equation.Practical implicationsThis is a simple and easy method of modification of methacrylate ester with phenyl groups to obtain a polymer of enhanced properties.Originality/valueThis is a novel method for enhancing the thermal as well as surface adhesion properties of methacrylate polymers which finds several applications in surface coatings and adhesives.


2017 ◽  
Vol 30 (7) ◽  
pp. 840-846 ◽  
Author(s):  
Jafar Rezania ◽  
Abbas Shockravi ◽  
Morteza Ehsani ◽  
Vahid Vatanpour

Three new organic-soluble polyimides (PIs) bearing flexible thioether linkages, thiazole, and pyridine ring units were synthesized from a novel thioether-bridged diamine monomer and commercially available aromatic dianhydrides (1–3) via chemical imidization method. The resulting polymers were obtained in high yields and possessed inherent viscosities in the range of 0.67–0.89. The PIs are characterized by Fourier-transform infrared (FTIR), nuclear magnetic resonance (NMR), differential scanning calorimetry, and thermogravimetric analysis (TGA). All of the PIs exhibited excellent solubility in polar solvent. The polymers showed good thermal stability with glass transition temperatures ( Tgs) in the range of 194–244°C, and decomposition temperatures ( T5%) exceeding 300°C were observed using TGA in nitrogen atmosphere for the current polymers.


e-Polymers ◽  
2008 ◽  
Vol 8 (1) ◽  
Author(s):  
Na Ying ◽  
Zhang Haibo ◽  
Zhang Yunhe ◽  
Niu Yaming ◽  
Jiang Sibo ◽  
...  

AbstractTwo novel poly (aryl ether ketone)s with anthracene moieties in the backbone were synthesized through the conventional nucleophilic aromatic substitution polycondensation for the first time, by using a new bisfluoro monomer, 9,10-bis(4-fluorobenzoyl) anthracene (AnBF). The structures of obtained polymers were confirmed by NMR, IR and UV characterizations. The polymers have high molecular weight and show good solubility in common organic solvents. Differential Scanning Calorimetry (DSC) indicates that they are vitrified polymers with high glass transition temperatures above 188° Thermogravimetric analysis (TGA) shows that these polymers have good thermal stability in nitrogen atmosphere with a 5% weight loss (TGA-5%) above 465°.


2020 ◽  
Vol 32 (8) ◽  
pp. 924-932
Author(s):  
Zhuwei Qin ◽  
Suyun Lv ◽  
Yixuan Wu ◽  
Cong Wang ◽  
Siyu Zhang ◽  
...  

A molecular theory design was carried out to synthesize a diamine monomer 1-(4-tert-butylphenyl)-1,1-bis[4-(4-aminophenoxy)] phenylethane containing tert-butyl, ether linkage, and triphenylmethane units. Then it was polymerized with several commercial aromatic dianhydrides, including diphenyl hexafluoroisopropylidene tetraic acid dianhydride (6FDA), diphenyl ether tetracarboxylic dianhydride (ODPA), biphenyltetracarboxylic dianhydride (BPDA), and benzophenone tetraacid dianhydride (BTDA), via the conventional two-step method to afford a series of aromatic polyimides (PIs). The structure and properties of the polymer were characterized by Fourier transform infrared (FTIR) spectroscopy, solubility test, thermogravimetric analysis, differential scanning calorimetry, ultraviolet–visible spectroscopy, and tensile tests. The results showed that there were characteristic peaks of PI around 1776, 1720, and 1378 cm−1 in the FTIR spectra; 6FDA-, ODPA-, and BPDA-based PI are easily soluble in N-methylpyrrolidone (NMP), concentrated sulfuric acid, N,N-dimethylacetamide (DMAc), pyridine, Tetrahydrofuran (THF), Trichloromethane (CHCl3), and other common organic solvents showing excellent solubility. In a nitrogen atmosphere, the glass transition temperature of the PI films are between 246°C and 275°C, the temperature of 5% weight loss is above 501°C, and the residual mass fraction at 750°C is 53–61%. The mechanical properties range from 67.2 MPa to 88.6 MPa. In addition to the BTDA-based PI film, the other three types of PI have good transparency. The simultaneous introduction of tert-butyl, ether linkages, and triphenylmethane units has a synergistic effect, which greatly improves the solubility of PI and maintains good thermal stability, mechanical properties, and optical properties of PI at the same time.


2001 ◽  
Vol 708 ◽  
Author(s):  
Seung-Hwan Lee ◽  
Akira Otomo ◽  
Tatsuo Nakahama ◽  
Toshiki Yamada ◽  
Shiyoshi Yokoyama ◽  
...  

ABSTRACTA novel rigid and planar chromophore, p-phenylene benzobisthiazole unit with donor and acceptor groups, has been synthesized for second-order nonlinear optical applications. The first hyperpolarizability, β, of the nonlinear optical (NLO) chromophore has been measured by a Hyper-Rayleigh Scattering technique at 1064 nm in 1,1,1,3,3,3-hexafluoro-2-propanol solution. The β value of the NLO chromophore is 405E-30 esu, which is about seventeen times that of the p-NA (nitroaniline) value. The chromophore showed good thermal stability up to 330 °C in nitrogen atmosphere.


2011 ◽  
Vol 19 (9) ◽  
pp. 763-772 ◽  
Author(s):  
P. Thiruvasagam ◽  
C. Shiva ◽  
C. Sundararaman ◽  
D. Venkatesan

New aromatic diimide-diol monomers were prepared by the aromatic nucleophilic substitution reaction of aromatic dianhydrides and 4-aminophenol/(4-aminophenyl)-2'-(4-hydroxy phenyl)propane. The monomers were characterized by IR and 1H-NMR spectroscopy. A series of poly(esterimide)s was prepared from diimide-diols and aromatic diacid chlorides by solution polycondensation reaction in N-methyl-2-pyrrolidone. The poly(esterimide)s were characterized by IR and 1H-NMR spectroscopy, X-ray diffraction, thermogravimetric analysis, differential scanning calorimetry, gel-permeation chromatography, solution viscosity and solubility behaviour. The poly(esterimide)s with flexible groups, methyl groups and 1,3-disubstituted phenyl rings in the chain were expected to disturb the symmetry, and their effects on the property were studied. Most of the poly(esterimide)s exhibited good solubility in common organic solvents. The poly(esterimide)s displayed good thermal stability, and the 10% weight loss under nitrogen atmosphere ranged from 361 to 439 °C respectively.


2017 ◽  
Vol 68 (8) ◽  
pp. 1895-1902
Author(s):  
Ioana Cristina Tita ◽  
Eleonora Marian ◽  
Bogdan Tita ◽  
Claudia Crina Toma ◽  
Laura Vicas

Thermal analysis is one of the most frequently used instrumental techniques in the pharmaceutical research, for the thermal characterization of different materials from solids to semi-solids, which are of pharmaceutical relevance. In this paper, simultaneous thermogravimetry/derivative thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC) were used for characterization of the thermal behaviour of candesartan cilexetil � active substance (C-AS) under dynamic nitrogen atmosphere and nonisothermal conditions, in comparison with pharmaceutical product containing the corresponding active substance. It was observed that the commercial samples showed a different thermal profile than the standard sample, caused by the presence of excipients in the pharmaceutical product and to possible interaction of these with the active substance. The Fourier transformed infrared spectroscopy (FT-IR) and X-ray powder diffraction (XRPD) were used as complementary techniques adequately implement and assist in interpretation of the thermal results. The main conclusion of this comparative study was that the TG/DTG and DSC curves, together with the FT-IR spectra, respectively X-ray difractograms constitute believe data for the discrimination between the pure substance and pharmaceutical forms.


Polymers ◽  
2021 ◽  
Vol 13 (4) ◽  
pp. 626
Author(s):  
Siti Hajar Mohamed ◽  
Md. Sohrab Hossain ◽  
Mohamad Haafiz Mohamad Kassim ◽  
Mardiana Idayu Ahmad ◽  
Fatehah Mohd Omar ◽  
...  

There is an interest in the sustainable utilization of waste cotton cloths because of their enormous volume of generation and high cellulose content. Waste cotton cloths generated are disposed of in a landfill, which causes environmental pollution and leads to the waste of useful resources. In the present study, cellulose nanocrystals (CNCs) were isolated from waste cotton cloths collected from a landfill. The waste cotton cloths collected from the landfill were sterilized and cleaned using supercritical CO2 (scCO2) technology. The cellulose was extracted from scCO2-treated waste cotton cloths using alkaline pulping and bleaching processes. Subsequently, the CNCs were isolated using the H2SO4 hydrolysis of cellulose. The isolated CNCs were analyzed to determine the morphological, chemical, thermal, and physical properties with various analytical methods, including attenuated total reflection-Fourier transform-infrared spectroscopy (ATR-FTIR), field-emission scanning electron microscopy (FE-SEM), energy-filtered transmission electron microscopy (EF-TEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). The results showed that the isolated CNCs had a needle-like structure with a length and diameter of 10–30 and 2–6 nm, respectively, and an aspect ratio of 5–15, respectively. Additionally, the isolated CNCs had a high crystallinity index with a good thermal stability. The findings of the present study revealed the potential of recycling waste cotton cloths to produce a value-added product.


2001 ◽  
Vol 666 ◽  
Author(s):  
Kazushige Ueda ◽  
Shin-ichiro Inoue ◽  
Sakyo Hirose ◽  
Hiroshi Kawazoe ◽  
Hideo Hosono

ABSTRACTMaterials design for transparent p-type conducting oxides was extended to oxysulfide system. LaCuOS was selected as a candidate for a transparent p-type semiconductor. It was found that the electrical conductivity of LaCuOS was p-type and controllable from semiconducting to semi-metallic states by substituting Sr2+ for La3+. LaCuOS films showed high transparency in the visible region, and the bandgap estimated was approximately 3.1 eV. Moreover, it was revealed that LaCuOS showed sharp excitonic absorption and emission at the bandgap edge, which is advantageous for optical applications. A layered oxysulfide, LaCuOS, was proposed to be a promising material for optoelectronic devices.


2013 ◽  
Vol 734-737 ◽  
pp. 2191-2194
Author(s):  
Li Li Wu ◽  
Yuan Lian ◽  
Dan Liu ◽  
Hua Zheng ◽  
Dian Wu Huang

In this study, flame retardant microcapsules were synthesized using magnesium hydroxide as core materials, melamine resin as the shell material. The structure, diameters and thermal properties of prepared microcapsules were investigated by using FTIR, ELS, DSC and TGA. The effects of core/shell ratio on the properties of microcapsules were studied.Flame retardant materials of low-density polyethylene/magnesium hydroxide microcapsules were prepared.The tensile strength and elongation at break tests were performed to determine its mechanical property.Inflammability of the materials was also studied.The results showed the prepared magnesium hydroxide microcapsule shows good thermal stability and it has free compatibility with the polymer.The composites of HDPE/MH microcapsules have good performance.


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