中文摘要 |
本研究以酚及福馬林為原料,三乙胺為催化劑,聚乙烯醇(Polyvinyl alcohol;PVA)為安定劑,六亞甲基四胺為架橋硬化劑,利用懸浮聚合法製造圓球狀PF樹脂粒子。反應過程包含三個階段,第一階段預聚合反應時,設定甲醛與酚之莫耳比為1.5/1,反應時間1.5、2.0及2.5 h。隨後加入不同種類及添加量之PVA使形成圓球狀樹脂粒子,最後加入六亞甲基四胺完成樹脂的硬化反應。由結果可知,預聚合反應時間1.5 h者較適合造粒反應,採用部分皂化PVA為安定劑者,所得圓球狀樹脂之粒徑較小;採用完全皂化PVA者,樹脂轉化率較高,所得圓球狀樹脂之粒徑較大。而隨PVA添加量增加,大尺寸粒子所佔比例減小。DSC熱分析顯示反應所得PF樹脂粒子已完全硬化。TGA熱分析顯示不同條件所製備圓球狀PF樹脂有相似之熱裂解行為,在加熱溫度430~600℃有較激烈之重量損失,而加熱至800℃之焦炭率約60%。
In this study, spherical phenol-formaldehyde (PF) resin beads were made by a suspension polymerization using phenol and formalin as raw materials, triethylamine, polyvinyl alcohol (PVA) and hexamethylene-tetramine as a catalyst, stabilizer and curing reagent, respectively. The reaction process consists of three stages. In the initial stage, the mixture of phenol and formaldehyde with a molar ratio of 1.5/1 was reacted for 1.5, 2.0 and 2.5 hours to undergo the pre-polymerization. After then, different kinds and dosages of PVA were added to form the spherical beads. Finally, hexamethylene-tetramine was added to complete the setting reaction of spherical PF resins. The results showed that the pre-polymerization with 1.5 hours was more adequate for the bead formation. Using the PVA with partially saponification as the stabilizer, the PF resin beads with a smaller diameter were obtained. While using the fully saponified PVA as the stabilizer, the higher degree of resin conversion rate and the larger diameter of resin beads were obtained. However, increasing the dosage of PVA added, the proportion of larger diameter beads would decrease. The result of DSC analysis showed that PF resin beads were fully cured. The result of TGA analysis indicated that PF resin beads prepared with different conditions had similar thermal degradation behavior. The drastic weight loss occurred at the temperature between 430℃ and 600℃. The char yield of these PF beads was about 60% at the temperature of 800℃. |