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At least 163 records · Page 9

A solvent resistant copolyimide

A solvent resistant copolyimide was prepared by reacting 4,4'-oxydiphthalic anhydride with a diamine blend comprising, based on the total amount of the diamine blend, about 75 to 90 mole percent of 3,4'-oxydianiline and about 10 to 25 mole percent p-phenylene diamine. The solvent resistant copolyimide had a higher glass transition temperature when cured at 350 C, 371 C and 400 C than LaRC(TM)-IA. The composite prepared from the copolyimide had similar mechanical properties to LaRC(TM)-IA. Films prepared from the copolyimide were resistant to immediate breakage when exposed to solvents such as dimethylacetamide and chloroform. The adhesive properties of the copolyimide were maintained even after testing at 23 C, 150 C, 177 C and 204 C.

Chang, Alice C.↗

Tough, soluble, aromatic, thermoplastic copolyimides

Tough, soluble, aromatic, thermoplastic copolyimides were prepared by reacting 4,4'-oxydiphthalic anhydride, 3,4,3',4'-biphenyltetracarboxylic dianhydride and 3,4'-oxydianiline. These copolyimides were found to be soluble in common amide solvents such as acetamide, Nmethylpyrrolidinone, and dimethylformamide allowing them to be applied as the fully imidized copolymer and to be used to prepare a wide range of articles.

Bryant, Robert G.↗

LaRC(TM)-IA Copolyimides

Copolyimides modified versions of LaRC(TM)-IA thermoplastic polyimide formulated by incorporating moieties of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and, alternatively, isophthaloyldiphthalic anhydride (IDPA) into LaRC(TM)-IA polymer backbones. Exhibit higher glass-transition temperatures and retain greater fractions of lower-temperature shear moduli at higher temperatures. Copolyimides spun into fibers or used as adhesives, molding powders, or matrix resins in many applications, especially in fabrication of strong, lightweight structural components of aircraft.

St. Clair, Terry L.↗

Crystalline imide/arylene ether copolymers

Crystalline imide/arylene ether block copolymers are prepared by reacting anhydride terminated poly(amic acids) with amine terminated poly)arylene ethers) in polar aprotic solvents and chemically or thermally cyclodehydrating the resulting intermediate poly(amic acids). The block copolymers of the invention have one glass transition temperature or two, depending on the particular structure and/or the compatibility of the block units. Most of these crystalline block copolymers for tough, solvent resistant films with high tensile properties. While all of the copolymers produced by the present invention are crystalline, testing reveals that copolymers with longer imide blocks or higher imide content have increased crystallinity.

Jensen, Brian J.↗

Processing and properties of fiber reinforced polymeric matrix composites: I. IM7/LARC(TM)-PETI-7 polyimide composites

A phenylethynyl terminated imide oligomer formed from the reaction of benzophenone tetracarboxylic acid dianhydride, an 75:25 molar ratio of 4,4'-oxydianiline and meta-phenylenediamine and 4-phenylethynylphthalic anhydride as the endcapper at a theoretical number average molecular weight (Mn) of approximately 3,700 g/mol was evaluated as a composite resin matrix. A glass transition temperature (Tg) of 315 deg C was reached after 250 deg C/1 hr annealing of the matrix resin. Unidirectional prepreg was made by coating an N-methylpyrrolidinone solution of the amide acid oligomer onto unsized IM7 graphite fibers. The thermal and rheological properties and the solvent/volatile depletion rates of the amide acid/NMP system were determined. This information was used to successfully design a molding cycle for composite fabrication. Composites molded under 800 Psi at 371 C consistently yielded good consolidation as measured by C-scan and optical photomicrography. The composite's short beam shear strength (SBS), longitudinal and transverse flexural strengths and moduli were measured at various temperatures. These composites exhibited excellent room temperature (RT) longitudinal flexural strength and modulus and RT SBS strength retention at 177 C.

Hou, Tan-Hung↗

A polyimide molecular composite

A polyimide is a hard and sturdy thermoplastic made from the combination of tetracarboxylic dianhydrides and diamines in a polar aprotic solvent. A series of polyimide blends comprising of a tough moldable, wholly aromatic polyimide and a highly crystalline rigid polyimide were prepared. The flexible polyimide was based on LaRC-SI with a 2% offset, and the rigid polyimide as based on para-phenylenediamine and biphenyltetracarboxylic dinnhydride encapped with pthalic anhydride. The polyimide blends were cast as films and cured at 100, 200, and 300 C in air. These films were characterized by finding their glass-transition temperature, melting temperature, coefficient of thermal expansion, tensile modulus, tensile strength, and percent elongation. These characterizations found out which polyimide blend had exceptional mechanical and thermal properties. Experimental results showed the following: (1) A blend with increasing amounts of flexible polyimide produced a better film; (2) A blend with increasing amounts of rigid polyimide produced a brittle film; (3) LaRC-SI (2% offset) tended to phase separate during film casting; (4) Most of the films produced were brittle; and (5) There was an inability to obtain mechanical and thermal properties due to having brittle film. These conclusions demonstrate the difficulty in producing a polyimide blend comprising two physically distinct polyimides. Combining a polysmide with a poly(amic acid) thermosett could be the next phase of research in polyimide synthesis.

Hart, Aprill J.↗

Process for Preparing a Tough, Soluble, Aromatic, Thermoplastic Copolyimide

A process for preparing a tough, soluble, aromatic, thermoplastic copolyimide is provided. The process comprises the steps of (a) providing 4.4'-oxydiphthalic anhydride to 3,4,3',4'-biphenyltetracarboxylic dianhydride at a mole ratio ranging from about 25 mole percent to 75 mole percent to 75 mole percent to about 25 mole percent; (b) adding 3,4'-oxydianiline to form a mixture; (c) adding a polar aprotic or polar protic solvent to the mixture to form a solution having a percentage of solids capable of maintaining polymer solubility; (d) stirring the solution to allow it to react; (e) adding an azeotropic solvent to the solution and heating to remove water; (f) cooling the solution of step (e) to room temperature and recovering the tough, soluble, aromatic, thermoplastic copolyimide.

Bryant, Robert G.↗

Organometallic Polymeric Conductors

For aerospace applications, the use of polymers can result in tremendous weight savings over metals. Suitable polymeric materials for some applications like EMI shielding, spacecraft grounding, and charge dissipation must combine high electrical conductivity with long-term environmental stability, good processability, and good mechanical properties. Recently, other investigators have reported hybrid films made from an electrically conductive polymer combined with insulating polymers. In all of these instances, the films were prepared by infiltrating an insulating polymer with a precursor for a conductive polymer (either polypyrrole or polythiophene), and oxidatively polymerizing the precursor in situ. The resulting composite films have good electrical conductivity, while overcoming the brittleness inherent in most conductive polymers. Many aerospace applications require a combination of properties. Thus, hybrid films made from polyimides or other engineering resins are of primary interest, but only if conductivities on the same order as those obtained with a polystyrene base could be obtained. Hence, a series of experiments was performed to optimize the conductivity of polyimide-based composite films. The polyimide base chosen for this study was Kapton. 3-MethylThiophene (3MT) was used for the conductive phase. Three processing variables were identified for producing these composite films, namely time, temperature, and oxidant concentration for the in situ oxidation. Statistically designed experiments were used to examine the effects of these variables and synergistic/interactive effects among variables on the electrical conductivity and mechanical strength of the films. Multiple linear regression analysis of the tensile data revealed that temperature and time have the greatest effect on maximum stress. The response surface of maximum stress vs. temperature and time (for oxidant concentration at 1.2 M) is shown. Conductivity of the composite films was measured for over 150 days in air at ambient temperature. The conductivity of the films dropped only half an order of magnitude in that time. Films aged under vacuum at ambient temperature diminished slightly in conductivity in the first day, but did not change thereafter. An experimental design approach will be applied to maximize the efficiency of the laboratory effort. The material properties (initial and long term) will also be monitored and assessed. The experimental results will add to the existing database for electrically conductive polymer materials. Attachments: 1) Synthesis Crystal Structure, and Polymerization of 1,2:5,6:9,10-Tribenzo-3,7,11,13-tetradehydro(14) annulene. 2) Reinvestigation of the Photocyclization of 1,4-Phenylene Bis(phenylmaleic anhydride): Preparation and Structure of (5)Helicene 5,6:9,10-Dianhydride. 3) Preparation and Structure Charecterization of a Platinum Catecholate Complex Containing Two 3-Ethynyltheophone Groups. and 4) Rigid-Rod Polymers Based on Noncoplanar 4,4'-Biphenyldiamines: A Review of Polymer Properties vs Configuration of Diamines.

Youngs, Wiley J.↗

Potentially Prebiotic Syntheses of Condensed Phosphates

In view of the importance of a prebiotic source of high energy phosphates, we have investigated a number of potentially prebiotic processes to produce condensed phosphates from orthophosphate and cyclic trimetaphosphate from tripolyphosphate. The reagents investigated include polymerizing nitriles, acid anhydrides, lactones, hexamethylene tetramine and carbon suboxide. A number of these processes give substantial yields of pyrophosphate from orthophosphate and trimetaphosphate from tripolyphosphate. Although these reactions may have been applicable in local areas, they are not sufficiently robust to have been of importance in the prebiotic open ocean.

Keefe, Anthony D.↗

Polyimide Fibers

A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and endcapped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340? C. to 360? C. and at heights of 100.5 inches, 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi; and a mean elongation in the range of 14 to 103%.

St.Clair, Terry L.↗

Tough, Soluble, Aromatic, Thermoplastic Copolyimides

Tough, soluble, aromatic, thermoplastic copolyimides were prepared by reacting 4,4'-oxydiphthalic anhydride, 3,4,3',4'-biphenyltetracarboxylic dianhydride and 3,4'-oxydianiline. These copolyimides were found to be soluble in common amide solvents such as N,N'-dimethyl acetamide, N-methylpyrrolidinone, and dimethylformamide allowing them to be applied as the fully imidized copolymer and to be used to prepare a wide range of articles.

Bryant, Robert G.↗

Polyimide Fibers

A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and end- capped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340 C. to 360 C. and at heights of 100.5 inches. 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi, and a mean elongation in the range of 14 to 103%.

St.Clair, Terry L.↗

IM7/LARC(tm) MPEI-1 Polymide Composites

LARC(Trademark) MPEI-1 (Langley Research Center(Trademark) modified phenylethynyl imide-1) phenylethynyl containing aromatic polymide, is based on the reaction of biphenyl dianhydride (BPDA), 3,4'-oxydianiline (3,4'-ODA), 1,3-bis(3-aminophenoxy)benzene (APB), 2,4,6-triaminopyrimidine (TAP) and 4-phenylethynyl phthalic anhydride (PEPA), presumably resulting in a mixture of linear, branched and star shaped phenylethynyl containing imides which was evaluated as a matrix for high-performance composites. The poly(amid acid) solution of MPEI-1 in N-methypyrrolidinone was synthesized at 35% and 42% solids. Unidirectional prepreg was fabricated from these solutions and Hercules IM7 carbon fiber utilizing NASA- Langley's multipurpose prepreg machine. The temperature-dependent volatile depletion rates, thermal crystallization behavior and resin theology were characterized. Based on this information, a composite molding cycle was developed which yielded well consolidated, void-free laminates. Composite mechanical properties such as short beam shear strength, longitudinal and transverse flexural strength and flexural modulus, longitudinal tensile strength and notched and unnotched compression strengths were measured at room temperature (RT) and elevated temperatures. These mechanical properties are compared with those of IM7/LARC(Trademark) PETI-5 composites.

Hou, T. H.↗

Phenylethynyl Containing Imide Oligomers

As part of a program to develop high performance/high temperature adhesives and composite matrices for a Mach 2.4 high speed civil transport, imide oligomers containing phenylethynyl groups were investigated. Phenylethynyl groups were placed on the ends of oligomers of different molecular weights (1250, 2500 and 5000 g/mol), pendent along the backbone of oligomers and both pendent and terminal on oligomers. Many different compositions of phenylethynyl containing imide oligomers had been previously prepared and evaluated before selecting the composition based upon 3,3'.4,4'-biphenyltetracarboxcylic dianhydride (BPDA), 3.4'-oxydianiline (3,4'-ODA) and 1,3-bis(3-aminophenoxy)benzene (APB) for extensive work. 4-Phenylethynylphthalic anhydride (PEPA) was used to place phenylethynyl groups on the ends of the oligomers and 3,5-diamino-4'-phenylethynylbenzophenone (DPEB) was used to introduce pendent phenylethynyl groups along the oligomeric backbone. Upon heating above 300 C, the phenylethynyl groups react to provide chain extension, branching and cross linking. Several of these materials exhibited excellent properties as adhesives and composite matrices. The chemistry, processability and properties of the oligomers, the cured polymers, bonded specimens and composites from phenylethynyl containing oligomers are presented.

Hergenrother, P. M.↗

Mechanical Characterization of Composites and Foams for Aerospace Applications

Experimental studies to investigate the mechanical properties of ultra-lightweight polyimide foams for space applications, compression after impact (CAI) properties for low velocity impact of sandwich composites, and aspen fiber/polypropylene composites containing an interface adhesive additive, Maleic Anhydride Grafted Polypropylene (MAPP), were performed at Clark Atlanta University. Tensile, compression, flexural, and shear modulus tests were performed on TEEK foams categorized by their densities and relative cost according to ASTM specifications. Results showed that the mechanical properties of the foams increased as a function of higher price and increasing density. The CAI properties of Nomex/phenolic honeycomb core, fiberglass/epoxy facesheet sandwich composites for two damage arrangements were compared using different levels of impact energy ranging from 0 - 452 Joules. Impact on the thin side showed slightly more retention of CAI strength at low impact levels, whereas higher residual compressive strength was observed from impact on the thick side at higher impact levels. The aspen fiber/polypropylene composites studied are composed of various percentages (by weight) of aspen fiber and polypropylene ranging from 30%-60% and 40%-100%, respectively. Results showed that the MAPP increases tensile and flexural strength, while having no significant influence on tensile and flexural modulus.

Veazie, D. R.↗

Method of Preparing Polymers with Low Melt Viscosity

This invention is an improvement in standard polymerizations procedures, i.e., addition-type and step-growth type polymerizations, wherein monomers are reacted to form a growing polymer chain. The improvement includes employing an effective amount of a trifunctional monomer (such as a trifunctional amine anhydride, or phenol) in the polymerization procedure to form a mixture of polymeric materials consisting of branced polymers, star-shaped polymers, and linear polymers. This mixture of polymeric materials has a lower melt temperature and a lower melt viscosity than corresponding linear polymeric materials of equivalent molecular weight.

Jensen, Brian J.↗

Method to Prepare Processable Polyimides with Non-Reactive Endgroups Using 1,3-bis(3-Aminophenoxy) Benzene

Polyimide copolymers were obtained containing 1,3-bis(3-aminophenoxy)benzene (APB) and other diamines and dianhydrides and terminating with the appropriate amount of a non-reactive endcapper, such as phthalic anhydride. Homopolymers containing only other diamines and dianhydrides which are not processable under conditions described previously can be made processable by incorporating various amounts of APB, depending on the chemical structures of the diamines and dianhydrides used. Polyimides that are more rigid in nature require more APB to impart processability than polyimides that are less rigid in nature. The copolymers that result from using APB to enhance processability have a unique combination of properties including excellent thin film properties, low pressure processing (200 psi and below), improved toughness, improved solvent resistance, improved adhesive properties, improved composite mechanical properties, long term melt stability (several hours at 390 C), and lower melt viscosities.

Jensen, Brian J.↗

Adhesive and Composite Properties of a New Phenylethynyl Terminated Imide

A relatively new phenylethynyl terminated imide oligomer (PETI) from the reaction of 2,3,',4'- biphenyltetracarboxylic dianhydride, 4,4'-oxydianiline and endcapped with 4- phenylethynylphthalic anhydride at a calculated number average molecular weight of 5000 g/mole was evaluated as an adhesive and composite matrix. The asymmetric dianhydride imparts a low melt viscosity to the oligomer and a high glass transition temperature to the cured resin. Preliminary adhesive work with titanium (6Al-4V) adherend gave good room temperature (RT) tensile shear strengths and excellent retention of RT strength at 260 C. Preliminary composite work using unsized IM7 carbon fiber provided moderate to high mechanical properties. The chemistry, mechanical, and physical properties of the new PETI in neat resin, adhesive and composite form are presented.

Thompson, C. M.↗