Characterization of Phenol-Formaldehyde Prepolymer Resins by In Line FT-IR Spectroscopy

Different resol phenol-formaldehyde prepolymer resins have been synthesized with different formaldehyde / phenol ratios. The phenolic resin composition depends on monomer ratio, catalyst, reaction conditions, and residual free monomers. Temperature and pH conditions under which reactions of phenols with formaldehyde are carried out have a profound effect on the characteristics of the resulting products. Three reaction sequences must be considered: formaldehyde addition to phenol, chain growth or prepolymer formation and finally the crosslinking or curing reaction. Two prepolymer types are obtained depending on pH, novolacs in an acidic pH region whereas resols by alkaline reaction. Resol resins are synthesized with a molar excess of formaldehyde (1<F/P<3). These are monoor polynuclear hydroxymethylphenols which are stable at room temperatures, but are transformed into three dimensional, cross linked, insoluble and infusible polymers by the application of heat. An ATR-FTIR spectrometry technique (ReactIR 4000) with light conduit and diamond-composite sensor was used to perform in-line monitoring of phenol-formaldehyde prepolymer synthesis. This technique was found to be ideal for determining residual free phenol and formaldehyde, individual phenol and formaldehyde conversions and prepolymer composition changes as a function of time when the condensation reaction was carried out. The kinetics data obtained through the ReactIR 4000 in-line reaction analysis system agreed well with those determined by the traditional titration method. ReactIR technology replaces time consuming and inaccurate off-line methodology.