In-situ characterization of the cure reaction of HTPB and IPDI by simultaneous NMR and IR measurements

Hailu, Kidist; Guthausen, Gisela; Becker, Wolfgang; König, Alexander M.; Bendfeld, A.; Geißler, Egon

doi:10.1016/j.polymertesting.2010.03.001

Cited by 73 publications

(56 citation statements)

References 13 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…However, NMR relaxation measurements have been proven to be readily applicable, for instance, for characterizing the state of a cured resin [106]. Relaxation measurements can be performed on solid surfaces and have been used to in-situ characterize the cure reaction of a polyurethane consisting of hydroxyl-terminated (poly)butadiene (HTPB) and isophorone diisocyanate (IPDI) monomers [13]. The authors applied NMR and IR measurements simultaneously.…”

Section: Other Online Monitoring Methodsmentioning

confidence: 99%

“…This indicates that silanized glass fibers (which are often used as reinforcement) have an influence on the composition of the cross-linked network by potentially forming a polystyrene-rich interphase of lower glass transition temperature in the region close to the reinforcement fiber [11]. Numerous other curing studies have been performed using FTIR realtime measurements, for instance, on epoxy resin cure [12] or polyurethane formation [13].…”

Section: General Aspects Instrumentationmentioning

confidence: 99%

See 1 more Smart Citation

Processing

Kandelbauer

2014

Handbook of Thermoset Plastics

View full text Add to dashboard Cite

Section: Other Online Monitoring Methodsmentioning

confidence: 99%

Section: General Aspects Instrumentationmentioning

confidence: 99%

Processing

Kandelbauer

2014

Handbook of Thermoset Plastics

View full text Add to dashboard Cite

“…(1). The kinetic analysis of this basic reaction has been carried out by using Fourier transform infrared (FTIR) spectroscopy [27,28], nuclear magnetic resonance (NMR) spectroscopy [28,29], differential scanning calorimetry (DSC) [30], sand rheological measurement [31,32].…”

Section: Adhesive Mechanismmentioning

confidence: 99%

Review of the Adhesively Bonded Interface in a Solid Rocket Motor

Zhou

Chen

et al. 2015

The Journal of Adhesion

View full text Add to dashboard Cite

One of the most challenging requirements in a solid rocket motor (SRM) is the integrity of the charge structure which is a multilayer adhesive joint involving the propellant, liner, and insulation. The propellant/liner/insulation interface is considered to be the weakest part of the whole structure. This interface has some of the usual features of an adhesively bonded interface, as well as its own special characteristics: the co-cured process, ingredient migration between interfaces, and complicated damage mechanisms. We give a technical and critical review of the past fifty years of existing research on many aspects of the propellant/liner/insulation interface in terms of the adhesive properties and adhesive mechanisms, ingredients migration, damage determination, and fracture analysis.To present a comprehensive outline of this interface we also clarify some remaining problems which should be addressed in the future. With significant improvements in the theoretical and experimental studies of the propellant/liner/insulation interface, the problem of integrity failure of the charge structure in SRM will be well resolved. Downloaded by [Cambridge University Library] at 07:15 14 August 2015 2

show abstract

“…For asymmetric diisocyanates, Speckhard et al 15 theoretically suggested that narrower sequence length distributions of hard segments are produced when increasing the ratios of rate constants between primary and secondary end groups. Similarly, Grepinet et al 17,18 estimated six different rate constants for reactions between 2,4-TDI and isomers with either 2-hydroxyethyl acrylate or PPG; and Hailu et al 19 determined four different rate constants for the reaction between isophorone diisocyanate (IPDI) and hydroxylterminated polybutadiene (HTPB). Similarly, Grepinet et al 17,18 estimated six different rate constants for reactions between 2,4-TDI and isomers with either 2-hydroxyethyl acrylate or PPG; and Hailu et al 19 determined four different rate constants for the reaction between isophorone diisocyanate (IPDI) and hydroxylterminated polybutadiene (HTPB).…”

Section: Introductionmentioning

confidence: 99%

Linear segmented polyurethanes: I. A kinetics study

Polo

Spontón

Jaramillo

et al. 2017

J of Applied Polymer Sci

View full text Add to dashboard Cite

This work investigates the two-step polymerization between methylene diphenyl diisocyanate (MDI), two different poly(tetramethylene oxide) macrodiols, and 1,4-butanediol (BD) as chain extender. At the end of the prepolymerization, the reaction mixture contains MDI in excess and a prepolymer with isocyanate end group. Then, BD and a solvent (tetrahydrofuran) were added to start the finishing stage under nominal stoichiometric equilibrium. The reaction was analyzed by Fourier transform infrared spectroscopy, hydrogen nuclear magnetic resonance ( 1 H-NMR), and size exclusion chromatography. 1 H-NMR was employed to follow global concentrations of unreacted isocyanate end groups and internal urethane groups. This information enabled to estimate the following "effective" rate constants: k 1 5 1.07 3 10 23 L mol 21 s 21 for the prepolymerization; and k 2 5 1.94 3 10 24 L mol 21 s 21 for the finishing stage. These values are subject to errors caused by biases introduced in the recipe, in the measurements, in the reaction conditions, in the quality of reagents, and in the reaction mechanism assumptions. Such errors also explain the dispersion of the published rate constants values. The 1 H-NMR measurements also enabled to estimate the evolution (with extent of reaction) of the numberaverage number of structural units along the prepolymerization and finishing stages; and such estimates reasonably verify Flory's classical expressions.

show abstract

In-situ characterization of the cure reaction of HTPB and IPDI by simultaneous NMR and IR measurements

Cited by 73 publications

References 13 publications

Processing

Processing

Review of the Adhesively Bonded Interface in a Solid Rocket Motor

Linear segmented polyurethanes: I. A kinetics study

Contact Info

Product

Resources

About