One-pot synthesis of semicrystalline polyamide imide based on 4,4’-diaminobenzanilide and 2,2-propylidene-bis(1,4-phenyleneoxy)diphthalic anhydride in molten benzoic acid

2018 ◽  
Vol 31 (1) ◽  
pp. 63-71 ◽  
Author(s):  
AE Soldatova ◽  
AY Tsegelskaya ◽  
GK Semenova ◽  
TS Kurkin ◽  
PV Dmitryakov ◽  
...  
Keyword(s):  
Molecular Weight ◽  
High Temperature ◽  
Benzoic Acid ◽  
High Molecular Weight ◽  
Scanning Calorimetry ◽  
One Pot ◽  
X Ray Scattering ◽  
Reactive Oligomer ◽  
Capillary Viscosimetry ◽  
Heating Up

High-temperature thermoplastic semicrystalline polyamide imide (PAI) with Tg = 250°C, and Tm = 370°C was synthesized from 4,4’-diaminobenzanilide, and 2,2-propylidene-bis (1,4-phenyleneoxy) diphthalic anhydride using three different methods: one-pot high-temperature catalytic polycondensation in molten benzoic acid (BA), low-temperature polycondensation (LTP) in dimethylacetamide (DMAA) followed by chemical imidization, and LTP followed by imidization. The influence of the synthetic route on the crystallinity of PAI was studied by wide-angle X-ray scattering. The PAI synthesized in molten BA comprised a reactive oligomer, which on heating up to 360°C easily transformed into high-molecular-weight PAI. The thermal and rheological properties of the high-molecular-weight PAI thus prepared were studied using differential scanning calorimetry, trimellitic acid, thermogravimetric analysis, and capillary viscosimetry. The rheological characteristics indicate that the obtained PAI can be melt processed by extrusion and hot pressing at 370–380°C.

scholarly journals Synthesis of High Molecular Weight Stereo-Di-Block Copolymers Driven by a Co-Initiator Free Catalyst

Polymers ◽  
2022 ◽  
Vol 14 (2) ◽  
pp. 232
Author(s):  
Carmen Moya-Lopez ◽  
Ivan Bravo ◽  
José A. Castro-Osma ◽  
David Chapron ◽  
Patrice Bourson ◽  
...  
Keyword(s):  
Molecular Weight ◽  
High Molecular Weight ◽  
Diblock Copolymers ◽  
Average Molecular Weight ◽  
Kinetic Studies ◽  
Scanning Calorimetry ◽  
One Pot ◽  
Mechanism Of Reaction ◽  
Sequential Addition ◽  
The One

Stereo-diblock copolymers of high molecular weight polylactide (PLA) were synthetized by the one pot-sequential addition method assisted by a heteroscorpionate catalyst without the need of a co-initiator. The alkyl zinc organometallic heteroscorpionate derivative (Zn(Et)(κ3-bpzteH)] (bpzteH = 2,2-bis(3,5-dimethylpyrazol-1-yl)-1-para-tolylethoxide) proved to assist in the mechanism of reaction following a coordination-insertion process. Kinetic studies along with the linear correlation between monomer and number average molecular weight (Mn) conversion, and the narrow polydispersities supported the truly living polymerization character of the initiator, whereas matrix-assisted laser desorption/Ionization-time of flight (MALDI-TOF) studies showed a very low order of transesterification. The high stereo-control attained for the afforded high molecular weight derivatives was revealed by homonuclear decoupled 1H NMR spectra and polarimetry measurements. The nanostructure of the PLA derivatives was studied by both wide-angle X-ray scattering (WAXS) and differential scanning calorimetry (DSC) and the stereocomplex phase of the PLA stereo-diblock copolymers was successfully identified.

scholarly journals Physicochemical and Antifungal Properties of Clotrimazole in Combination with High-Molecular Weight Chitosan as a Multifunctional Excipient

Marine Drugs ◽  
2020 ◽  
Vol 18 (12) ◽  
pp. 591
Author(s):  
Bożena Grimling ◽  
Bożena Karolewicz ◽  
Urszula Nawrot ◽  
Katarzyna Włodarczyk ◽  
Agata Górniak
Keyword(s):  
Molecular Weight ◽  
High Molecular Weight ◽  
Weight Ratio ◽  
Scanning Calorimetry ◽  
Minimal Inhibitory Concentrations ◽  
Dissolution Tests ◽  
Effective Combination ◽  
The Impact ◽  
High Molecular Weight Chitosan

Chitosans represent a group of multifunctional drug excipients. Here, we aimed to estimate the impact of high-molecular weight chitosan on the physicochemical properties of clotrimazole–chitosan solid mixtures (CL–CH), prepared by grinding and kneading methods. We characterised these formulas by infrared spectroscopy, differential scanning calorimetry, and powder X-ray diffractometry, and performed in vitro clotrimazole dissolution tests. Additionally, we examined the antifungal activity of clotrimazole–chitosan mixtures against clinical Candida isolates under neutral and acid conditions. The synergistic effect of clotrimazole and chitosan S combinations was observed in tests carried out at pH 4 on Candida glabrata strains. The inhibition of C. glabrata growth reached at least 90%, regardless of the drug/excipient weight ratio, and even at half of the minimal inhibitory concentrations of clotrimazole. Our results demonstrate that clotrimazole and high-molecular weight chitosan could be an effective combination in a topical antifungal formulation, as chitosan acts synergistically with clotrimazole against non-albicans candida strains.

Ultra high molecular weight polyethylene with improved plasticity and toughness by high temperature melting

Polymer ◽  
2010 ◽  
Vol 51 (12) ◽  
pp. 2721-2731 ◽  
Author(s):  
Jun Fu ◽  
Bassem W. Ghali ◽  
Andrew J. Lozynsky ◽  
Ebru Oral ◽  
Orhun K. Muratoglu
Keyword(s):  
Molecular Weight ◽  
High Temperature ◽  
High Molecular Weight ◽  
Ultra High Molecular Weight ◽  
Temperature Melting

Stereocomplex electrospun fibers from high molecular weight of poly(L-lactic acid) and poly(D-lactic acid)

2020 ◽  
Vol 40 (2) ◽  
pp. 136-142 ◽  
Author(s):  
Homa Maleki ◽  
Hossein Barani
Keyword(s):  
Molecular Weight ◽  
Lactic Acid ◽  
Thermal Properties ◽  
High Molecular Weight ◽  
Chemical Properties ◽  
Electrospun Fibers ◽  
Scanning Calorimetry ◽  
Force Microscopy ◽  
Atomic Force ◽  
Electrospinning Method

AbstractThe stereocomplex formation is a promising method to improve the properties of poly(lactide) (PLA)-based products due to the strong interaction of the side-by-side arrangement of the molecular chains. Recently, electrospinning method has been applied to prepare PLA stereocomplex, which is more convenient. The objective of the current study is to make stereocomplexed PLA nanofibers using electrospinning method and compare their properties and structures with pure poly(l-lactide) (PLLA) fibers. The stereocomplexed fibers were electrospun from a blend solution of high molecular weight PLLA and poly(d-lactide) (1:1 ratio). The morphology of the obtained electrospun fibers was examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Differential scanning calorimetry was applied to study their thermal properties and crystallinity. Fourier transform infrared spectroscopy (FTIR) test was conducted on the samples to characterize their chemical properties. The SEM and AFM images indicated that smooth uniform fibers with a cylindrical structure were produced. Besides, the FTIR results and thermal properties confirmed that only stereocomplex crystallites formed in the resulting fibers via the electrospinning method.

Synthesis of Segmented Anisotropic-Isotropic Poly(Aryl Ester)Poly(Arylene Ether) Copolymers

1989 ◽  
Vol 175 ◽  
Author(s):  
J. E. McGratn ◽  
K. L. Cooper ◽  
W. Waehamad ◽  
H. Huang ◽  
G. L. Wilkes
Keyword(s):  
Molecular Weight ◽  
Liquid Crystal ◽  
Benzoic Acid ◽  
Liquid Crystalline ◽  
Average Molecular Weight ◽  
Nucleophilic Aromatic Substitution ◽  
Copolymer Composition ◽  
Aromatic Substitution ◽  
Scanning Calorimetry ◽  
Arylene Ether

AbstractCarboxyl functional poly(arylene ether) oligomers of controlled number average molecular weight were synthesized via nucleophilic aromatic substitution step polymerization using p-hydroxy benzoic acid as the molecular weight and end group controlling reagents. The subsequent functionalized polyarylene ethers were copolymerized with acetoxy benzoic acid or acetoxyphenoxy benzoic acid via melt acidolysis procedures. Successful copolymers were generated using chlorobenzene as a solvent for the first s age of the reaction followed by melt reaction at temperatures as high as 325°C. Resulting copolymer composition and segment size were investigated. It was possible to prepare improved solvent resistant copolymers through incorporation of the liquid crystal polyester (LCP) segment. Extraction tests using boiling chloroform showed that a high percentage of segmented copolymer were generated. Swelling characteristics were also noted and were observed to decrease as a function of the LCP concentration utilized. Multiple transitions were observed in differential scanning calorimetry consistent with Tg's, Tm's and possibly with liquid crystal transitions. Optical microscopy showed an ordered microstructure developed which is consistent with the presence of liquid crystalline phases. The materials were successfully compression molded to afford tough coherent films at all compositions, implying the likelihood of improved compressive strength relative to the LCP homo- or copolyesters.

In Situ High Temperature X-Ray Diffraction Studies of Modified Poly(Ethylene Terephthalate)

1992 ◽  
Vol 36 ◽  
pp. 379-386
Author(s):  
T. Blanton ◽  
R. Seyler
Keyword(s):  
High Temperature ◽  
Ethylene Terephthalate ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
X Ray Scattering ◽  
Poly Ethylene Terephthalate ◽  
Poly Ethylene ◽  
Pet Crystallization

The effect of dimethyl-5-sodiosulfoisophthalate, SIP, on poly(ethylene terephthalate), PET, crystallization has been studied using in situ high-temperature x-ray diffraction, HTXRD. At low levels of SIP modification, PET-like crystallinity was observed. At high SIP levels, clustering of polyester ionomers was observed and crystallization was significantly suppressed. The HTXRD data along with differential scanning calorimetry, DSC, and small angle x-ray scattering, SAXS, indicate that the change from bulk crystallization to bulk ionomer formation occurred when 8-12 mol% of the diester linkages contained SIP.

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.

High Molecular Weight Polyethylene Nanospheres: Synthesis Physical and Mechanical Properties

2008 ◽  
Vol 8 (6) ◽  
pp. 3123-3135 ◽  
Author(s):  
Pradip Paik ◽  
Kamal K. Kar
Keyword(s):  
Mechanical Properties ◽  
Molecular Weight ◽  
Particle Size ◽  
Electron Microscope ◽  
Elastic Modulus ◽  
High Molecular Weight ◽  
Melting Temperature ◽  
Ion Beam ◽  
Atomic Scale ◽  
Scanning Calorimetry

The high molecular weight (MW) polyethylene (PE) particles of particle size varied from macro to micron to nanometer were synthesized by Grignard reagent. The microscopy analysis (scanning electron microscope, SEM; transmission electron microscope, TEM; and atomic force microscope, AFM) shows the spherical shape of PE particles. The effects of particle size, varies from macro to nanometer scale on crystal structure, crystallinity (χc), glass transition temperature (Tg), melting temperature (Tm), surface roughness and mechanical properties were studied. Differential scanning calorimetry (DSC) experiments show that the nanoparticles of PE are highly crystalline (χc ≈ 72%). The crystal length of PE nanoparticles is found to be approximately 14 Å. Although the Gibbs-Thomson equation is explained the depression of melting temperature (ΔTm) by 5 °C, the impervious results of Tg are still not fully understood. The low roughness value (2 Å) proves the presence of "atomic-scale-chain" folding at the surface of PE nanoparticles. A novel protocol is developed, and the elastic modulus of individual nanospherical PE particles is computed from 'force-distance' mapping curves of AFM. Hemispherical tungsten (W) tip was fabricated from focused ion beam and used as an indenter to measure the mechanical properties. It is found that the nano sized PE particles have higher elastic modulus (E = 1.2–1.4 GPa) compared to the bulk or macro sized PE (E = 0.6–0.7 GPa). The results corroborate the robustness of our experiments, since, the analogous results for macro sized particles match well with the literature.

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