Synergistic interaction of renewable nipagin and eugenol for high performance aromatic copoly(ether ester) materials

Abstract Naturally occurring nipagin and eugenol were used as the collaborative starting materials for poly(ether ester) materials. In this study, two series of nipagin and eugenol-derived copoly(ether ester)s, PHN11-xE1x and PHN11-xE2x (x = 0%, 5%, 10%, 15%, 20%), were prepared with renewable 1,6-hexanediol as a comonomer. The nipagin-derived component acts as the renewable surrogate of petroleum-based dimethyl terephthalate (DMT), while the eugenol-derived component acts as the cooperative property modifier of parent homopoly(ether ester) PHN1. 1,6-Hexanediol was chosen as the spacer because of its renewability and short chain to enhance the glass transition temperatures (Tgs) of materials. The molecular weights and chemical structures were confirmed by gel permeation chromatograph (GPC), NMR and FTIR spectroscopies. Thermal and crystalline properties were studied by thermal gravimetric analysis (TGA), differential scanning calorimetric (DSC) and wide-angle X-ray diffraction (WXRD). The tensile assays were conducted to evaluate the mechanical properties. The results suggest that properties of such kind of poly(ether ester)s can be finely tuned by the relative content of two components. Synergistic interaction of two structurally distinctive parts endows the materials with high performance.

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Synergistic interaction of renewable nipagin and eugenol for aromatic copoly(ether ester) materials with desired performance

Scientific Reports ◽

10.1038/s41598-021-03614-z ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Keling Hu ◽

Huachao Sui ◽

Dongping Zhao

Keyword(s):

Differential Scanning Calorimetric ◽

Gravimetric Analysis ◽

X Ray Diffraction ◽

Polybutylene Terephthalate ◽

X Ray ◽

Molecular Weights ◽

Chemical Structures ◽

Naturally Occurring ◽

High Boiling Point ◽

Ether Ester

AbstractNaturally occurring nipagin and eugenol were used as the collaborative starting materials for poly(ether ester) polymers. In this study, two series of nipagin and eugenol-derived copoly(ether ester)s, PHN11−xE1x and PHN11−xE2x (x = 0%, 5%, 10%, 15%, 20%), were prepared with renewable 1,6-hexanediol as a comonomer. The nipagin-derived component acts as the renewable surrogate of petroleum-based dimethyl terephthalate (DMT), while the eugenol-derived component acts as the cooperative property modifier of parent homopoly(ether ester) PHN1. 1,6-Hexanediol was chosen as the spacer because of its renewability, high boiling point, and short chain to enhance the glass transition temperatures (Tgs) of materials. The molecular weights and chemical structures were confirmed by gel permeation chromatograph (GPC), NMR and FTIR spectroscopies. Thermal and crystalline properties were studied by thermal gravimetric analysis (TGA), differential scanning calorimetric (DSC) and wide-angle X-ray diffraction (WXRD). The tensile assays were conducted to evaluate the mechanical properties. The results suggested that properties of this kind of poly(ether ester)s could be finely tuned by the relative content of two components for the desired applications (elastomer, rubbery) suitable for different scenarios from polyethylene glycol terephthalate (PET) and polybutylene terephthalate (PBT).

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Phenylethynyl-terminated oligoimides with ultra-low melt viscosity derived from 1,4-bis(3,4-dicarboxy phenoxy)benzene dianhydride

High Performance Polymers ◽

10.1177/0954008319832347 ◽

2019 ◽

Vol 31 (5) ◽

pp. 580-589 ◽

Cited By ~ 1

Author(s):

Wei Wang ◽

Guofei Chen ◽

Xingzhong Fang

Keyword(s):

Mechanical Properties ◽

Mechanical Analysis ◽

X Ray Diffraction ◽

Aromatic Diamines ◽

Melt Viscosity ◽

X Ray ◽

Good Thermal Stability ◽

Molecular Weights ◽

Chemical Structures ◽

Very High

Most of the existing polyimide oligomers for resin transfer molding (RTM) processing exhibited high melt viscosity, which can only maintain below 1 Pa·s at 280°C for 2 h, leading to very high process temperatures. So novel RTM-type oligomers with lower and stable melt viscosities are more desirable. Three series of thermoset oligoimides derived from 1,4-bis(3,4-dicarboxy phenoxy)benzene dianhydride and three different aromatic diamines were prepared herein. The diamines included 4,4′-oxydianiline, 2,2′-bis(trifluoromethyl)benzidine (TFDB), and 2-phenyl-4,4′-diaminodiphenyl ether ( p-ODA). 4-Phenylethynylphthalic anhydride was used as an endcapping reagent. Effects of the chemical structures and molecular weights of the oligoimides on their aggregated structures, melt processability, and the thermal and mechanical properties of the cured films were then systematically investigated. X-Ray diffraction results indicated that ODA series oligoimides and TFDB series oligoimides showed crystallinity in various degrees. However, the asymmetric p-ODA enables the p-ODA series oligoimides to exhibit amorphous forms. It was found that the p-ODA-based oligoimide with a molecular weight of 750 g mol−1 showed very low melt viscosity of 1 Pa·s even at 210°C, and the melt viscosity could maintain below 1 Pa·s after isothermal aging for 2 h at any temperature in the range of 200–280°C by rheological measurements. The cured film also showed a high glass transition temperature of 355°C by dynamic mechanical analysis, very good thermal stability by thermogravimetric analysis, and good mechanical properties. It might be more suitable for RTM processes in the future.

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Bio-Based Aromatic Copolyesters: Influence of Chemical Microstructures on Thermal and Crystalline Properties

Polymers ◽

10.3390/polym12040829 ◽

2020 ◽

Vol 12 (4) ◽

pp. 829

Author(s):

Keling Hu

Keyword(s):

High Performance ◽

Polymer Chains ◽

Polymer Materials ◽

Size Exclusion ◽

Differential Scanning Calorimetric ◽

Average Weight ◽

Gravimetric Analysis ◽

Excellent Thermal Stability ◽

Future Design ◽

Chemical Structures

Aromatic copolyesters, derived from bio-based nipagin and eugenol, were synthesized with renewable 1,6-hexandiol as the spacer. Number-average, weight-average molecular weights (Mn, Mw), and polydispersity (D) values were determined by size exclusion chromatography (SEC). Chemical structures were confirmed by 1H NMR and 13C NMR spectroscopies. Chemical microstructure analysis suggested that the nipagin and eugenol-derived units were inserted into polymer chains in an arbitrary manner. Due to the short chain of 1,6-hexanediol, the splitting of magnetically different methylene carbons, adjacent to the alcohol-oxygens, proved to be more sensitive towards sequence distributions, at the dyed level, than those from 1,10-decanediol. Thermal gravimetric analysis (TGA) demonstrated that these polyester materials have excellent thermal stability (>360 °C), regardless of the content of eugenol-derived composition incorporated. Differential scanning calorimetric (DSC) and wide-angle X-ray diffraction (WXRD) experiments revealed the semicrystalline nature for this kind of copolyesters. The crystallinities gradually decreased with the increase of eugenol-derived composition. Thermal and crystalline properties were well discussed from the microscopic perspective. The point of this work lies in establishing guidance for future design and modification of high-performance polymer materials from the microscopic perspective.

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High Yield Polyborosilazane Precursor for SiBN Ceramics

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.1004-1005.409 ◽

2014 ◽

Vol 1004-1005 ◽

pp. 409-414 ◽

Cited By ~ 4

Author(s):

Shuai Yong Jin ◽

Kang Kang Guo ◽

Hui Min Qi ◽

Ya Ping Zhu ◽

Fan Wang

Keyword(s):

Photoelectron Spectroscopy ◽

High Yield ◽

Cross Linking ◽

Differential Scanning Calorimetric ◽

Gravimetric Analysis ◽

Thermal Gravimetric ◽

X Ray Diffraction ◽

Ceramic Yield ◽

X Ray ◽

Amorphous Structures

The processible and high yield polyborosilazane (PBSZ) precursor for SiBN ceramics was prepared by coammonolysis reaction of dichlorosilane and trichloroborazine. The synthesized PBSZ precursor was characterized by Fourier Transform Infrared spectroscopy (FTIR),1H,11B, and29Si Nuclear Magnetic Resonance (NMR), and its ceramic conversion chemistry was investigated by differential scanning calorimetric (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and thermal gravimetric analysis (TGA). The PBSZ precursor is a viscous liquid and changes to an insoluble solid via a cross-linking reaction between the N-H group and Si-H group as post-heated from 60 to 180°C. The insoluble solid is transformed to Si3N4and BN amorphous structures with an approximately 95% ceramic yield after being pyrolyzed to 1000°C.

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High Resolution Replication of Organoclay Surfaces

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100055126 ◽

1982 ◽

Vol 40 ◽

pp. 576-577

Author(s):

W. W. Barker ◽

W. E. Rigsby ◽

V. J. Hurst ◽

W. J. Humphreys

Keyword(s):

Clay Mineral ◽

Organic Molecule ◽

Organic Molecules ◽

X Ray Diffraction ◽

Xrd Pattern ◽

X Ray ◽

Naturally Occurring ◽

Silicate Layers ◽

Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

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Hydrochloric Acid Modification and Lead Removal Studies on Naturally Occurring Zeolites from Nevada, New Mexico, and Arizona

Processes ◽

10.3390/pr9071238 ◽

2021 ◽

Vol 9 (7) ◽

pp. 1238

Author(s):

Garven M. Huntley ◽

Rudy L. Luck ◽

Michael E. Mullins ◽

Nick K. Newberry

Keyword(s):

New Mexico ◽

Surface Area ◽

Bet Surface Area ◽

Lead Removal ◽

X Ray Diffraction ◽

Sem Images ◽

X Ray ◽

Naturally Occurring ◽

27Al Mas Nmr ◽

Modified Zeolites

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.

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New Haloterpenes from the Marine Red Alga Laurencia papillosa: Structure Elucidation and Biological Activity

Marine Drugs ◽

10.3390/md19010035 ◽

2021 ◽

Vol 19 (1) ◽

pp. 35

Author(s):

Mohamed Shaaban ◽

Ghada S. E. Abou-El-Wafa ◽

Christopher Golz ◽

Hartmut Laatsch

Keyword(s):

Biological Activity ◽

Crude Extract ◽

Structure Elucidation ◽

Antimicrobial Activities ◽

Red Alga ◽

Spectroscopic Methods ◽

X Ray Diffraction ◽

X Ray ◽

Chemical Structures ◽

Terpene Derivatives

Analysis of the air-dried marine red alga Laurencia papillosa, collected near Ras-Bakr at the Suez gulf (Red Sea) in Egypt delivered five new halogenated terpene derivatives: aplysiolic acid (1), 7-acetyl-aplysiol (2), aplysiol-7-one (3), 11,14-dihydroaplysia-5,11,14,15-tetrol (5a), and a new maneonene derivative 6, named 5-epi-maneolactone. The chemical structures of these metabolites were characterized employing spectroscopic methods, and the relative and absolute configurations were determined by comparison of experimental and ab initio-calculated NMR, NOE, ECD, and ORD data, and by X-ray diffraction of 2 and 6. The antimicrobial activities of the crude extract and compounds 1–3, 5a and 6 were studied.

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Enhancement of Chloroprene/Natural/Butadiene Rubber Nanocomposite Properties Using Organoclays and Their Combination with Carbon Black as Fillers

Polymers ◽

10.3390/polym13071085 ◽

2021 ◽

Vol 13 (7) ◽

pp. 1085

Author(s):

Patricia Castaño-Rivera ◽

Isabel Calle-Holguín ◽

Johanna Castaño ◽

Gustavo Cabrera-Barjas ◽

Karen Galvez-Garrido ◽

...

Keyword(s):

Mechanical Properties ◽

Carbon Black ◽

High Performance ◽

Rubber Matrix ◽

Butadiene Rubber ◽

X Ray Diffraction ◽

X Ray ◽

Rubber Blends ◽

Ft Ir ◽

Chloroprene Rubber

Organoclay nanoparticles (Cloisite® C10A, Cloisite® C15) and their combination with carbon black (N330) were studied as fillers in chloroprene/natural/butadiene rubber blends to prepare nanocomposites. The effect of filler type and load on the physical mechanical properties of nanocomposites was determined and correlated with its structure, compatibility and cure properties using Fourier Transformed Infrared (FT-IR), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and rheometric analysis. Physical mechanical properties were improved by organoclays at 5–7 phr. Nanocomposites with organoclays exhibited a remarkable increase up to 46% in abrasion resistance. The improvement in properties was attributed to good organoclay dispersion in the rubber matrix and to the compatibility between them and the chloroprene rubber. Carbon black at a 40 phr load was not the optimal concentration to interact with organoclays. The present study confirmed that organoclays can be a reinforcing filler for high performance applications in rubber nanocomposites.

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Rapid four-component synthesis of dihydropyrano[2,3-c]pyrazoles using nano-eggshell/Ti(IV) as a highly compatible natural based catalyst

BMC Chemistry ◽

10.1186/s13065-021-00734-5 ◽

2021 ◽

Vol 15 (1) ◽

Author(s):

Arefeh Dehghani Tafti ◽

Bi Bi Fatemeh Mirjalili ◽

Abdolhamid Bamoniri ◽

Naeimeh Salehi

Keyword(s):

Thermo Gravimetric Analysis ◽

Reaction Times ◽

Diffraction Field ◽

Gravimetric Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Solvent Free Conditions ◽

High Yields ◽

Work Up

AbstractNano-eggshell/Ti(IV) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives. The characterization of nano-eggshell/Ti(IV) was performed using Fourier Transform Infrared spectroscopy, X-ray Diffraction, Field Emission Scanning Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and Thermo Gravimetric Analysis. Dihydropyrano[2,3-c]pyrazoles were synthesized in the presence of nano-eggshell/Ti(IV) via a four component reaction of aldehydes, ethyl acetoacetate, malononitrile and hydrazine hydrate at room temperature under solvent free conditions. The principal affairs of this procedure are mild condition, short reaction times, easy work-up, high yields, reusability of the catalyst and the absence of toxic organic solvents.

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Enhanced Photocatalytic Activity of Cu2O Cabbage/RGO Nanocomposites under Visible Light Irradiation

Polymers ◽

10.3390/polym13111712 ◽

2021 ◽

Vol 13 (11) ◽

pp. 1712

Author(s):

Appusamy Muthukrishnaraj ◽

Salma Ahmed Al-Zahrani ◽

Ahmed Al Otaibi ◽

Semmedu Selvaraj Kalaivani ◽

Ayyar Manikandan ◽

...

Keyword(s):

Electron Microscopy ◽

Thermo Gravimetric Analysis ◽

Visible Region ◽

Catalytic Performance ◽

Precipitation Method ◽

Gravimetric Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Dye Pollutants ◽

Transmission Electron

Towards the utilization of Cu2O nanomaterial for the degradation of industrial dye pollutants such as methylene blue and methyl orange, the graphene-incorporated Cu2O nanocomposites (GCC) were developed via a precipitation method. Using Hummers method, the grapheme oxide (GO) was initially synthesized. The varying weight percentages (1–4 wt %) of GO was incorporated along with the precipitation of Cu2O catalyst. Various characterization techniques such as Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), UV–visible diffused reflectance (UV-DRS), Raman spectroscopy, thermo gravimetric analysis (TGA), energy-dispersive X-ray analysis (EDX), and electro chemical impedance (EIS) were followed for characterization. The cabbage-like morphology of the developed Cu2O and its composites were ascertained from field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM). In addition, the growth mechanism was also proposed. The results infer that 2 wt % GO-incorporated Cu2O composites shows the highest value of degradation efficiency (97.9% and 96.1%) for MB and MO at 160 and 220 min, respectively. Further, its catalytic performance over visible region (red shift) was also enhanced to an appreciable extent, when compared with that of other samples.

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