Thermal degradation and curing of polyphenylene
Polyphenylene thermal degradation and curing, discussing pyrolytic effects of chlorine and polynuclear structure
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Polyphenylene thermal degradation and curing, discussing pyrolytic effects of chlorine and polynuclear structure
Three aromatic diamines have properties that make them promising candidates as curing agents for converting isocyanates to polyurethanes with higher adhesive strengths, higher softening temperatures, better toughness, and improved abrasion resistance.
Detailed data are presented on phenolic-glass and phenolic-asbestos compounds which compare the effect of compression molding without degas to the effects of four variations of compression molding. These variations were designed to improve elimination of entrapped volatiles and the volatile products of the condensate reaction associated with the cure of phenolic resins. The utilization of conventional methods of degas plus degas by vacuum and directional heat flow methods are involved. Detailed data are also presented on these same compounds, comparing the effect of changes in post-bake time, and post-bake temperature for the five molding techniques.
An approach for the development of a practical low temperature (293 K-311 K/68 F-100 F) curing adhesive system based on a family of amide/ester resins was studied and demonstrated. The work was conducted on resin optimization and adhesive compounding studies. An improved preparative method was demonstrated which involved the reaction of an amine-alcohol precursor, in a DMF solution with acid chloride. Experimental studies indicated that an adhesive formulation containing aluminum powder provided the best performance when used in conjunction with a commercial primer.
Fourteen ether-containing, aromatic dianhydrides have been synthesized from N-phenyl-3 or 4-nitrophthalimide and various bisphenols. The process involves nucleophilic displacement of activated nitro groups with bisphenolate ions. Ether-containing dianhydrides were indefinitely stable in the presence of atmospheric moisture. One-step, high temperature solution polymerization of the ether-containing dianhydrides with m-phenylene diamine, 4,4'-oxydianiline and 1, 3-bis(4-aminophenoxy)benzene afforded 42 polyetherimides. The polyetherimides were all soluble in m-cresol except two which were found to be crystalline. The glass transition temperatures of the polyetherimides ranged from 178 to 277 C. Soluble polybenzimidazopyrrolones containing ether groups were also prepared from the same ether-containing dianhydrides and aromatic tetraamines by one-step solution polymerization. Using low molecular weight polyetherimides, various thermoset resin systems were developed and tested as matrices for fiber-reinforced composites. The curing chemistry involving reaction of the phthalonitrile group and the o-diaminophenyl group was found to be generally applicable to crosslinking various aromatic polymers other than polyimides.
Report describes work with concentrations down to 0.07 percent and is useful when applying adhesives in terrestrial and space applications. Cured Silicone retains low-outgassing properties as well as its snap, elongation, and resilience. Tests for hardness of silicone material also showed good results. No gross hysteresis observable on recovery from stretching nor was there any decrease in hardness.
Finely-woven nylon cloth that has been treated with Teflon improves vacuum adhesive bonding of coatings to substrates. Cloth is placed over coating; entire assembly, including substrate, coating, and cloth, is placed in plastic vacuum bag for curing. Cloth allows coating to "breathe" when bag is evacuated. Applications include bonding film coatings to solar concentrators and collectors.
Thermal mechanical analysis was employed to monitor the penetration temperature of a low-temperature epoxy resin. Both neat resin and E-glass composite samples were examined. The effects of cure temperature variation and moisture content on the apparent glass transition temperature were determined.
The invention relates to reaction cured glass and glass coatings prepared by reacting a compound selected from the group consisting of silicon tetraboride, silicon hexaboride, other boron silicides, boron and mixtures with a reactive glass frit composed of a porous high silica borosilicate glass and boron oxide. The glassy composites of the present invention are useful as coatings on low density fibrous porous silica insulations used as heat shields and for articles such as reaction vessels that are subjected to high temperatures with rapid heating and cooling and that require resistance to temperature and repeated thermal shock at temperatures up to about 1482C (2700PF).
Chemical formulation produces foamed polyimide plastic without externalheat. Foam is less dense and more flame and acid resistant than conventional polyimide foams. Self curing foam can be formed "onsite" in limitedaccess locations where application of heat is difficult or impossible.
Tiles of space shuttle reusable surface insulation coated with reaction cured glass were subjected to 25 cycles of launch pad exposure and simulated mission heating. The coating could not withstand the environment without cracking. Water absorption after cracking reached as high as 150 weight percent. Exposure of insulation fibers beneath the coating to contaminants dissolved in absorbed water initiated fiber degradation.
Thermal mechanical analysis was employed to monitor the penetration temperature of a low-temperature epoxy resin (EPON 826/D230). Both neat resin and E-glass composite samples were examined. The effects of cure temperature variation and moisture content on the apparent glass transition temperature were determined.
Two improved cure-in-place silicone-elastomer-based adhesives have low thermal expansion and low thermal conductivity. Adhesives are flexible at low temperature and withstand high temperatures without disintegrating. New ablative compounds were initially developed for in-flight repair of insulating tile on Space Shuttle orbiter. Could find use in other applications requiring high-performance adhesives, such as sealants for solar collectors.
Delamination problem in reinforced carbon/carbon parts impregnated with oxalic acid-catalyzed furfuryl alcohol overcome by instituting two additional quality-control tests on alcohol and by changing curing conditions.
Curing epoxy resins with novalac phenolic resins is a feasible approach for increasing intact char of the resin system. Char yields above 40% at 700 C were achieved with epoxy novalac (DEN 438)/novalac phenolic (BRWE 5833) resin systems with or without catalyst such as ethyl tri-phenyl phosphonium iodide. These char yields are comparable to commercially used epoxy resin systems like MY-720/DDS/BF3. Stable prepregs are easily made from a solvent solution of the epoxy/phenolic system and this provides a feasible process for fabrication of same into commercial laminates.
A study was made on the cure kinetics of an epoxy neat-resin (Narmco 5208) using Differential Scanning Calorimetry (DSC). Two interrelated analytical methods were applied to dynamic DSC data for evaluating the kinetic parameters, such as activation energy, E, the order of reaction, n, and the total heat of polymerization (or crosslinking), delta H sub t. The first method was proposed by Ellerstein (1968), and uses a thorough differential-integral analysis of a single DSC curve to evaluate the kinetic parameters. The second method was proposed by Kissinger (1957), and uses multiple DSC curves obtained at various heating rates to evaluate E regardless of n. Kinetic analysis of Narmco 5208 epoxy resin showed that the reaction order, n, is substantially affected by the rate of heating; i.e., n is approximately 2 at slow scan rates but is reduced to 1.5 at higher scan rates. The activation energy, E, is not affected by the scan rate, and the average value of E is 25.6 + or - 1.8 kcal/mole.
Key reaction parameters estimated from single run. Single DSC Curve used to construct linearized plot from which kinetic reaction parameters are obtained: vertical axis intercept proportional to activation energy, while slope equals reaction order. DSC methods show promise for rapid screening and estimation of cure kinetic parameters of epoxy resins.
Partial substitution of a p-aminostyrene end-cap for the monomethyl ester of 5-norbornene-2, 3-dicarboxylic acid lowered the final cure temperature of typical PMR resins from 600 F to 500 F. The weight loss characteristics of neat resins and graphite fiber composites prepared by using the mixed end-cap approach were determined at 600 F. The room temperature and short-time elevated temperature mechanical properties of the composites at 550 F and 600 F were determined. The mechanical property retention characteristics of the composites at 550 F and 600 F are discussed.