化工学院 优秀毕业设计—环氧树脂阻燃剂的合成及表征.doc

环氧树脂阻燃剂的合成及表征 摘 要 DOPO（9，10-2氢-9-氧-10磷杂菲-10-氧化物）和4HBA（4-羟基苯甲醛）通过加成反应合成DOPO-HB(2-6-氧-6-氢-二苯并磷氧杂-6-酮4-羟基苯甲醇Synthesis and Characterization of Epoxy Resin Flame Retardant Abstract A novel phosphorus-containing hydroxyl benzoaldehyde (DOPO-HB) from 9,10-dihydro-9-oxa-10– phosphaphenanthrene -10-oxide (DOPO) and 4-hydroxyl benzoaldehyde was obtained via simple addition reactions.The synthesis conditions of DOPO-HB were also optimized A novel phosphorous -containing flame retardants 10-(2,5-dicarbonylpropyl) 9,10-dihydro-9-oxa-10-phospha- phenanthrene-10- oxide (DOPO-ITA) was synthesized using 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO) and itaconic acid(ITA) as starting materials.The chemical structure of the obtained DOPO-HB and DOPO-ITA were characterized with FTIR, 1H and 31P NMR and elemental analysis. The DOPO-HB, with multi-phenol groups in the molecular chain, was used as a poly functional curing agent for epoxies. The activity and activation energies of the DOPO-HB curing reactions with epoxies were investigated with differential scanning calorimetry (DSC). The thermal properties and thermal degradation behaviors of the DOPO-HB-cured epoxy resins were also studied with DSC and thermo gravimetric analysis(TGA). The paper also focuses on the solubility of DOPO-HB in different solvents with the temperature trend, the results show that, the solubility of DOPO-HB in benzene, toluene and xylene, and water increases with the temperature rising. Moreover, the benzene xylene toluene Water Keywords: Epoxy resin Curing agent Flame retardant solubility 目 录 摘 要 I Abstract II 1 绪 论 1 1.1 阻燃问题的提出 1 1.2阻燃技术发展概述 1 1.3磷系阻燃剂概述 2 1.4磷系阻燃剂阻燃机理 3 1.5磷系阻燃剂的研究 4 1.6前人的工作成果 5 1.7本论文的可行性研究 7 1.8本论文研究的主要内容 7 2 DOPO-HB的合成 8 2.1 前言 8 2.2 合成方法 8 2.3 实验部分 8 2.3.1 实验试剂 8 2.3.2 实验仪器 8 2.3.3 实验步骤 9 2.3.4实验流程图 10 2.4 DOPO-HB的表征 10 2.4.1 TGA 10 2.4.2 DSC 11 2.4.3 熔点 12 2.4.4 红外光谱 12 2.5 小结 13 3 DOPO-HB溶解度的测定 14 3.1概述 14 3.2实验部分 14 3.2.1.溶解度测定实验仪器 14 3.2.2实验步骤 14 3.2.3.实验装置 1