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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Direct Synthesis of Polyester from Biomass Derived 1,6-hexanediol using a Copper-Ceria Catalyst

Biomass derived polyesters are gaining attention due to their increased mechanical and thermal properties, and also because of their biodegradability. These polyesters are typically synthesized from polycondensation reactions between diols with dicarboxylic acids using catalysts. Other methods such as alcoholysis and acidolysis of low molecular weight esters and alcoholysis of acyl chlorides are also well known. Direct conversion of diol to ester without using dicarboxylic acid is not well known, and to our knowledge has not been reported over a solid catalyst. In this study, we report a direct synthesis of polyester from 1,6-hexanediol using a copper-ceria catalyst without using a dicarboxylic acid monomer. The copper-ceria catalysts were synthesized by incipient wetness impregnation method and characterized using X-ray photoelectron spectroscopy (XPS), X-ray diffraction analysis (XRD), Brunauer-Emmett-Teller (BET), and infrared spectroscopy (IR). Our initial studies show that 1,6-hexanediol can be converted to corresponding polyester at higher temperatures under atmospheric pressures of CO2 or N2. The reaction products were analyzed using nuclear magnetic resonance spectroscopy (NMR), gel permeation chromatography (GPC), high performance liquid chromatography (HPLC), and IR spectroscopy.

Biomass derived diols↗
DOE OSTI2024

Lignin molecular weights of Populus trichocarpa residues after CELF pretreatment

Here we present a dataset of molecular weights of lignin from a woody energy crop (Populus trichocarpa) residues after a series of co-solvent enhanced lignocellulosic fractionation (CELF) pretreatment. The natural poplar variant GW-9947 from the Center for Bioenergy Innovation (CBI) was used. The poplar was knife milled and passed through a 1 mm sieve and CELF pretreatment was performed in a Parr autoclave reactor with 7.5 wt % solids loading, 0.5 wt% H2SO4 as catalyst at 150°C with various time. Tetrahydrofuran was added in a 1:1 mass ratio with water as the pretreatment solvent. Lignin was isolated from the pretreated samples after ball-milling in a porcelain jar with ceramic balls via Retsch PM 200 at 580 rpm for 2.5 h followed by enzymatic hydrolysis in acetate buffer (pH 4.8, 50 °C) for 48 h. The solid residue was isolated by centrifugation and hydrolyzed again with freshly added buffer and enzymes for another 48 h. After filtration, the solid residue was extracted twice with 96% (v/v) 1,4-dioxane/water mixture at room temperature overnight. The extracts were combined, rotary evaporated, and freeze-dried to recover lignin. The lignin samples were then derivatized in an acetic anhydride/pyridine (1:1, v/v) mixture and stirred at room temperature for 24 h. Ethanol was added to the reaction mixture, left for 30 min and then removed with a rotary evaporator. The addition and removal of ethanol was repeated at least 3 times until all traces of acetic acid were removed. Acetylated lignin samples were then dissolved in tetrahydrofuran (THF) at a concentration of 1.0 mg/mL. The molecular weight of acetylated lignin was measured by a gel permeation chromatography (GPC) on a PSS-Polymer Standards Service (Warwick, RI, USA) GPC SECurity 1200 system featuring Agilent HPLC 1200 components equipped with four Waters Styragel columns (HR1, HR2, HR4 and HR6) and an UV detector (270 nm). Tetrahydrofuran was used as the mobile phase and flow rate was 0.3 mL/min. The Polymer Standards Service WinGPC Unity software (Build 6807) was used for data processing for all the samples. The data provides information about the effects of CELF pretreatment time at 150 ºC on lignin molecular weights.

09 BIOMASS FUELS↗
DOE OSTI2024

Characterization of Levan Fructan Produced by a Gluconobacter japonicus Strain Isolated from a Sugarcane Processing Facility

During raw sugarcane processing, a significant portion of lost sucrose is attributable to microbial degradation. Sucrose consumption by many bacteria is also linked to the production of exopolysaccharides (EPS) such as dextrans and fructans. These resulting EPS cause operational challenges during raw sugar manufacturing. Here, we report the characterization of EPS from a fructan-forming Gluconobacter japonicus bacterium that we previously isolated from a Louisiana sugarcane factory. The genome sequencing revealed the presence of two encoded levansucrase genes, lsrA and lsrB. One levansucrase, LsrB, was detected in the secreted protein fraction of G. japonicus LASM12 by QTOF LC-MS. The spotting assays indicated that G. japonicus produces EPS using sucrose and raffinose as substrates. The G. japonicus EPS correlated with levan fructan commercial standards by 1H-NMR, and with the characteristic carbohydrate fingerprint region for FTIR spectra, confirming that the G. japonicus EPS is levan fructan. The glycosyl composition and glycosyl linkage analysis revealed a linear β-2,6-fructofuranosyl polysaccharide with occasional (5.7%) β-2,1-fructofuranosyl branches. The gel permeation chromatography of the levan fructan EPS showed two main peaks at 4.5 kDa and 8 kDa and a very minor peak at 500 kDa. G. japonicus was identified as a producer of levan fructan. These findings will be useful for future studies aimed at evaluating the impact of levan fructans on sugar crop processing, which have been historically underestimated in industry.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Synthesis and Characterization of Copolymers and Nanocomposites from Limonene, Styrene and Organomodified-Clay Using Ultrasonic Assisted Method

In the present work, we report a simple synthesis method for preparation of copolymers and nanocomposites from limonene and styrene using clay as a catalyst. The copolymerization reaction is carried out by using a proton exchanged clay as a catalyst called Mag-H+. The effect of temperature, reaction time and amount of catalyst were studied, and the obtained copolymer structure (lim-co-sty) is characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy (1H-NMR) and differential scanning calorimetry (DSC). The molecular weight of the obtained copolymer is determined by gel permeation chromatography (GPC) and is about 4500 g·mol−1. The (lim-co-sty/Mag 1%, 3%, 7% and 10% by weight of clay) nanocomposites were prepared through polymer/clay mixture in solution method using ultrasonic irradiation, in the presence of Mag-CTA+ as green nano-reinforcing filler. The Mag-CTA+ is organophilic silicate clay prepared through a direct exchange process, using cetyltrimethylammonuim bromide (CTAB). The prepared lim-co-sty/Mag nanocomposites have been extensively characterized by FT-IR spectroscopy, X-ray diffraction (XRD), scanning electronic microscopy (SEM) and transmission electronic microscopy (TEM). TEM analysis confirms the results obtained by XRD and clearly show that the obtained nanocomposites are partially exfoliated for the lower amount of clay (1% and 3% wt) and intercalated for higher amounts of clay (7% and 10% wt). Moreover, thermogravimetric analysis (TGA) indicated an enhancement of thermal stability of nanocomposites compared with the pure copolymer.

Derdar, Hodhaifa↗
DOE OSTI2025

Enabling Industrial Re-Use of Large-Format Additive Manufacturing Molding and Tooling

Large-format additive manufacturing (LFAM) is an enabling manufacturing technology capable of producing large parts with highly complex geometries for a wide variety of applications, including automotive, infrastructure/construction, and aerospace mold and tooling. In the past decade, the LFAM industry has seen widespread use of bio-based, glass, and/or carbon fiber reinforced thermoplastic composites which, when printed, serve as a lower-cost alternative to metallic parts. One of the highest-volume materials utilized by the industry is carbon fiber (CF)-filled polycarbonate (PC), which in out-of-autoclave applications can achieve comparable mechanical performance to metal at a significantly lower cost. Previous work has shown that if this material is recovered at various points throughout the manufacturing process for both the lab and pilot scale, it can be mechanically recycled with minimal impacts on the functional performance and printability of the material while significantly reducing the feedstock costs. End-of-life (EOL) CF-PC components were processed through industrial shredding, melt compounding, and LFAM equipment, followed by evaluation of the second-life material properties. Experimental assessments included quantitative analysis of fiber length attrition, polymer molecular weight degradation using gel permeation chromatography (GPC), density changes via pycnometry, thermal performance using dynamic mechanical analysis (DMA), and mechanical performance (tensile properties) in both the X- and Z-directions. Results demonstrated a 24.6% reduction in average fiber length compared to virgin prints, accompanied by a 21% decrease in X-direction tensile strength and a 39% reduction in tensile modulus. Despite these reductions, Z-direction tensile modulus improved by 4%, density increased by 6.8%, and heat deflection temperature (HDT) under high stress retained over 97% of its original value. These findings underscore the potential for integrating mechanically recycled CF-PC into industrial LFAM applications while highlighting the need for technological innovations to mitigate fiber degradation and enhance material performance for broader adoption. This critical step toward circular material practices in LFAM offers a pathway to reducing feedstock costs and environmental impact while maintaining functional performance in industrial applications.

additive manufacturing↗
NASA NTRS1971

Long-term aging of elastomers: Chemical stress relaxation of fluorosilicone rubber and other studies

Aerospace applications of elastomers are considered, including: propellant binders, bladder materials for liquid propellant expulsion systems, and fuel tank sealants for high-speed aircraft. A comprehensive molecular theory for mechanical properties of these materials has been developed but has only been tested experimentally in cases where chemical degradation processes are excluded. Hence, a study is being conducted to ascertain the nature, extent, and rate of chemical changes that take place in some elastomers of interest. Chemical changes that may take place in the fluorosilicone elastomer, LS 420, which is regarded as a fuel and high-temperature-resistant rubber are investigated. The kinetic analysis of the chemical stress relaxation and gel permeation chromatography studies comprise the major portion of the report.

Kalfayan, S. H.↗
NASA NTRS1972

Long Term Aging of Elastomers: Chemorheology of Viton B Fluorocarbon Elastomer

The continuation of a study to ascertain the nature, extent, and the rate of chemical changes that take place in certain selected elastomers is reported. Under discussion is Viton B, regarded as a temperature and fuel resistant fluorocarbon rubber. The kinetic analysis of the chemical stress relaxation, and infrared and gel permeation chromatography analysis results are discussed.

Kalfayan, S. H.↗
NASA NTRS1972

Hydrocarbon polymeric binder for advanced solid propellant

A series of DEAB initiated isoprene polymerizations were run in the 5-gallon stirred autoclave reactor. Polymerization run parameters such as initiator concentration and feed rate were correlated with the molecular weight to provide a basis for molecular weight control in future runs. Synthetic methods were developed for the preparation of n-1,3-alkadienes. By these methods, 1,3-nonadiene was polymerized using DEAB initiator to give an ester-telechelic polynonadiene. This was subsequently hydrogenated with copper chromite catalyst to give a hydroxyl terminated saturated liquid hydrocarbon prepolymer having greatly improved viscosity characteristics and a Tg 18 degrees lower than that of the hydrogenated polyisoprenes. The hydroxyl-telechelic saturated polymers prepared by the hydrogenolysis of ester-telechelic polyisoprene were reached with diisocyanates under conditions favoring linear chain extension gel permeation chromatography was used to monitor this condensation polymerization. Fractions having molecular weights above one million were produced.

Potts, J. E.↗
NASA NTRS1973

Poly/diphenylsiloxy/arylazines. I - Synthesis and characterization

A detailed description is presented for the synthesis of poly(diphenylsiloxy)arylazines by the melt polymerization of hydroxyarylazines and bis(anilino)diphenylsilane. The resulting polymers have been characterized by elemental analysis, gel-permeation chromatography, vapor-phase osmometry, and UV-VIS-IR optical spectroscopy.

Goldsberry, R. E.↗
NASA NTRS1976

Accelerated heat-aging studies on fluororubber in various media

Heat-aging studies were conducted on fluororubber (copolymers of vinylidene fluoride and perfluoropropylene) using N,N-dicinnamylidene-1,6-hexanediamine, a Schiff's base of 1,6-hexanediamine, and MgO as acid acceptor. The principal technique employed was chemical stress relaxation for determining network changes brought about in the heat-aged fluororubber. This technique was backed up by swelling measurements, gel permeation chromatography, and IR spectroscopy. Stress relaxation curves are plotted for a wide range of variation in parameters (time, crosslinking density, state of curing, temperature, intermittent and continuous relaxation).

Kalfayan, S. H.↗
NASA NTRS1977

Distribution of molecular weight in glyceride polymerizates or aggregates of them after contact with lunar grains

An attempt is made to report on experiments in which a molecular-weight increase was determined in thin layers of triglyceride-containing glycerides after thin-layer contact for two years with lunar topsoil grains at 25 C without any thermal activation. It is noted that solidification was observed on both dielectric grains and metal-rich areas and that changes in viscosity and molecular weights were first detected by solidification of surface layers. Gel permeation chromatography is described which detected a general shift of the Gaussian distribution of the molecular-weight data toward generally higher molecular weights as well as an increase in mean molecular weight. Reaction mechanisms are considered, and results of spectrographic analysis are cited which support the interpretations of the molecular-weight data.

Asunmaa, S. K.↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

By varying the stoichiometry of the reactants in the preparation of PMR polyimide resin, changes occur in molecular weight distribution which influence the rheological properties and thus the processability of the resin, as well as the mechanical properties of the composite. The influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system were exposed. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F, glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

This preliminary study explores the influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1981

Benzoic acid degradation of polyacrylonitrile fibers

The reactions of polyacrylonitrile (PAN) fibers in the presence of benzoic acid have been studied. Polyacrylonitrile fibers oxidize more readily in the presence of benzoic acid than in air at temperatures in the range of 170 C. The product decreased in solubility with extent of reaction. Gel permeation chromatography of the soluble fraction showed change in polydispersity. The insoluble product exhibited differences in weight loss as a function of decomposition temperature compared to PAN fibers. Infrared analyses of the fiber product showed absorption peaks similar to air-oxidized PAN. High-energy photoelectron spectral analysis showed a carbon-rich surface which contained oxygen and nitrogen. An air oxidized sample of fiber contained more oxygen at the surface than a fiber treated first with benzoic acid and then air oxidized.

Varma, D. S.↗
NASA NTRS1981

Benzoic acid degradation of polyacrylonitrile fibers

The reactions of polyacrylonitrile (PAN) fibers in the presence of benzoic acid have been studied. Polyacrylonitrile fibers oxidize more readily in the presence of benzoic acid than in air at temperatures in the range of 170 C. The product decreased in solubility with extent of reaction. Gel permeation chromatography of the soluble fraction showed change in polydispersity. The insoluble product exhibited differences in weight loss as a function of decomposition temperature compared to PAN fibers. Infrared analyses of the fiber product showed absorption peaks similar to air-oxidized PAN. High-energy photoelectron spectral analysis showed a carbon-rich surface which contained oxygen and nitrogen. An air oxidized sample of fiber contained more oxygen at the surface than a fiber treated first with benzoic acid and then air oxidized.

Varma, D. S.↗
NASA NTRS1982

Ultrahigh molecular weight aromatic siloxane polymers

The condensation of a diol with a silane in toluene yields a silphenylene-siloxane polymer. The reaction of stiochiometric amounts of the diol and silane produced products with molecular weights in the range 2.0 - 6.0 x 10 to the 5th power. The molecular weight of the product was greatly increased by a multistep technique. The methodology for synthesis of high molecular weight polymers using a two step procedure was refined. Polymers with weight average molecular weights in excess of 1.0 x 10 to the 6th power produced by this method. Two more reactive silanes, bis(pyrrolidinyl)dimethylsilane and bis(gamma butyrolactam)dimethylsilane, are compared with the dimethyleminodimethylsilane in ability to advance the molecular weight of the prepolymer. The polymers produced are characterized by intrinsic viscosity in tetrahydrofuran. Weight and number average molecular weights and polydispersity are determined by gel permeation chromatography.

Ludwick, L. M.↗
NASA NTRS1984

Bioassay, isolation and studies on the mechanism of action of neurite extension factor

The identification and purification of molecules active in promoting neurite outgrowth requires a sensitive reproducible bioassay. A quantitative bioassay was utilized to purify a neurite extension factor (NEF) based on counting the number of phase bright neurons with processes at least equal to one cell body diameter after 20 hrs. in culture is defined, serum free medium. Using a combination of heat treatment DEAE cellulose chromatography and gel filtration, an acidic protein of M sub r = 75,000 was highly purified. Upon reduction, it yields subunits of M sub r = 37,000. Purified fractions are active half maximally at 100 ng/ml in inducing neurite outgrowth in this bioassay. Currently, monoclonal antibodies to NEF are being produced. Female Balb C mice were immunized with the antigen and fusions with mouse myeloma cells will be performed to yield hybridoma cells.

Kligman, D.↗