Phenol-urea-formaldehyde (PUF) resins were synthesized by reacting mixture of methylolureas (MMU), phenol, and formaldehyde. The structure of PUF cocondensed resins at different stages of reaction were analyzed by liquid 13C nuclear magnetic resonance (NMR) spectroscopy. The liquid 13C-NMR analysis indicated that methylolureas had the dominant content in MMU with the reaction between urea and formaldehyde under the alkaline condition. The PUF cocondensed resins had no free formaldehyde. methylolureas were well incorporated into the cocondensed resins by reacting with phenolic units to form cocondensed methylene bridges. The second formaldehyde influenced the further reaction and the structure of the PUF resins. The resins with the prepared method of PUFB possessed relatively high degree of polymerization and low proportion of unreacted methylol groups. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009
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