基于淀粉液化的APF树脂的合成及表征  

Synthesis and characterization of APF resin based on liquified amylum

作　　者：王凯伦 刘雪纯 甘卫星 张晨晨 农光再 陈绪高 张一甫 WANG Kai-lun;LIU Xue-chun;GAN Wei-xing;ZHANG Chen-chen;NONG Guang-zai;CHEN Xu-gao;ZHANG Yi-fu(School of Resources, Environment and Materials, Guangxi University, Nanning 530004,China)

机构地区：[1]广西大学资源环境与材料学院

出　　处：《桂林理工大学学报》2019年第2期446-452,共7页Journal of Guilin University of Technology

基　　金：国家自然科学基金项目(31360158);国家科技支撑计划项目(2015BAD14B03);广西科技重大专项(桂科AA17204067;桂科AA16380051)

摘　　要：以淀粉、苯酚、甲醛为主要原料合成液化淀粉改性酚醛树脂(APF),对APF树脂的合成工艺及性能进行探讨,并分析液化产物及APF树脂的分子结构,测定APF树脂的分子量。正交试验表明,APF树脂的最佳合成工艺为甲醛与苯酚的摩尔比为1.6∶1,苯酚与淀粉的质量比为2.0∶1,氢氧化钠与苯酚的摩尔比为0.375∶1。在此条件下,胶合强度为1.061 MPa,储存期可达69 d(25℃),液化残渣率仅为0.174%。FT-IR分析结果表明:液化阶段淀粉水解生成葡萄糖和少部分5-羟甲基糠醛,并与苯酚形成芳基醚键结构;合成阶段芳基醚键断裂,苯酚优先羟甲基化,葡萄糖或5-羟甲基糠醛可能在羟甲基苯酚的邻位和对位发生缩聚或缩醛反应生成APF树脂。GPC测试结果表明APF树脂的数均分子量为1 271。The modified phenolic resin based on liquified amylum(APF) was synthesized from starch, phenol and formaldehyde. While saving production cost, the formaldehyde release of plywood is reduced, which is beneficial to ecological and environmental protection. The synthesis technology and properties of APF resin were discussed and the molecular structure of the liquified product and APF resin were analyzed. The molecular weight of APF resin was determined. Orthogonal experiments showed that the formaldehyde to phenol mole ratio of 1.6, the phenol to starch mass ratio of 2 and the sodium hydroxide to phenol molar ratio of 0.375 were the best synthesis process of APF resin. The booding strength of APF resin was 1.061 MPa, the storage life can be up to 69 days at the temperature of 25 ℃, and the liquefaction residue rate was only 0.17%. The results of FT-IR analysis showed that amylum was hydrolyzed during the liquefaction stage to produce glucose and part of 5-HMF, and formed an aryl ether bond structure with phenol. In the synthesis stage, the aromatic ether bond fracture, phenol priority methylation, glucose or 5-HMF may be in the neighborhood and position of hydroxymethyl phenol condensation or acetal reaction to produce APF resin. The results of GPC analysis showed that the average molecular weight of APF resin was 1 271.

关 键 词：APF树脂 正交实验 FT-IR GPC 

分 类 号：TQ32[化学工程—合成树脂塑料工业]