Formaldehyde resins, molecular weight characterization

Molecular Weight Characterization of Resole Phenol—Formaldehyde Resins... 

Dase-catalyzed phenol-formaldehyde resins polymerized with a mole ratio of formaldehyde to phenol greater than one pose an interesting molecular weight characterization problem. This system is a dynamic one with active methylol end groups. Branched and crosslinked structures are formed, and in general, the separation of the resin from the reaction mixture is difficult. Figure 1 illustrates the chemical nature of a resole resin. 

Various ionization methods were used to bombard phenol-formaldehyde oligomers in mass spectroscopic analysis. The molecular weights of resole resins were calculated using field desorption mass spectroscopy of acetyl-derivatized samples.74 Phenol acetylation was used to enable quantitative characterization of all molecular fractions by increasing the molecular weights in increments of 42. 

Copolymer resin (p-CAF) was synthesized by the condensation of p-cresol and adipamide with formaldehyde in the presence of hydrochloric acid as catalyst and using varied molar ratios of reacting monomers. A composition of the copolymers has been determined on the basis of their elemental analysis. The number average molecular weight of resins was determined by conductometric titration in non-aqueous medium. The copolymer resins were characterized by viscometric measurements in dimethylsulphoxide (DMSO), UV-visible absorption spectra in non-aqueous medium, infrared (IR) spectra, and nuclear magnetic resonance (NMR) spectra. The morphology of the copolymers was studied by scanning electron microscopy (SEM). 

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