水溶性环己酮-三聚氰胺-甲醛共缩聚树脂的合成与表征

Synthesis and Characterization of Water-Soluble Cyclohexanone-Melamine-Formaldehyde Resin

以环己酮、三聚氰胺、甲醛为原料,氢氧化钠为催化剂,用"两步法"合成出环己酮-三聚氰胺-甲醛树脂(CMFR),考察了三聚氰胺用量、醛酮物质的量比、催化剂用量及反应时间等对CMFR的游离甲醛含量及溶水倍数的影响,并借助FT-IR、13C-NMR、DSC、TG等对CMFR进行了表征。发现在环己酮、三聚氰胺、甲醛物质的量比为1.0∶0.2∶2.0,催化剂用量为0.6%,反应时间为120min,反应温度为90℃的条件下,合成出的CMFR游离甲醛含量为0.45%,溶水倍数为8.2。FT-IR和13C-NMR结果表明CMFR分子中存在三聚氰胺结构;DSC分析表明CMFR仅存在一个固化放热峰,说明三聚氰胺参与了树脂的共缩聚反应,形成了均一的分子结构,其固化温度约为182.5℃,固化后CMFR的耐溶剂性能提高。

The eyclohexanone-melamine-formaldehyde resin （CMFR） was synthesized by a two-step method with cyclohexanone, melamine and formaldehyde as raw materials and sodium hydroxide as catalyst. The effects of melamine dosage, molar ratio of aldehyde to ketone, and reaction time on the free formaldehyde content and water solubilization multiple of CMFR were investigated. The resin was characterized by FT-IR, 13C-NMR, DSC and TG. It was found that the content of free formaldehyde in CMFR was 0.45% and the water solubilization multiple was 8.2 when the molar ratio of cyclohexanone to melamine to formaldehyde was 1.0：0.2：2.0, the amount of catalyst was 0.6% , the reaction time and temperature was 120min and 90℃ respectively. The results of FT-IR and ^13C-NMR showed that there was a melamine structure in the CMFR molecule. The DSC analysis showed that there was only one peak of curing exothermic peak in CMFR. It was indicated that the melamine had participated in the co-polyeondensation and formed a homogeneous molecular structure; and the curing temperature of the resin was 182.5℃; and the solvent resistance of CMFR had improved after curing.