13C-NMR analysis of phenol-urea-formaldehyde prepolymers and phenol-urea-formaldehyde-tannin adhesives

Abstract

Phenol-urea-formaldehyde-tannin (PUFT) adhesives were prepared by co-polymerization of Pinus pinaster bark tannins with phenol-urea-formaldehyde (PUF) prepolymers at room temperature. A detailed analysis by ¹³C-NMR spectroscopy of the resins together with an evaluation of their properties was performed in order to find suitable preparation conditions for prepolymers prior to their co-polymerization with tannins. ¹³C-NMR spectroscopy allowed identification of the different linkages formed and quantification of the main functional groups in the PUF prepolymers, which were greatly influenced by the preparation conditions. The decrease in the free formaldehyde content in the PUFT adhesives with respect to the original prepolymers was attributed to tannin methylolation at room temperature. The fast increase in the apparent viscosity of the PUFT adhesives after the blending suggested the possibility of a co-polymerization reaction between tannins and the PUF prepolymers; however, the occurrence of this reaction could not be confirmed by ¹³C-NMR.

Keywords:

• 13 C-NMR
• PINUS PINASTER BARK TANNINS
• PUF PREPOLYMERS
• TANNIN-MODIFIED ADHESIVES