摘要本课题采用季戊四醇、三氯氧磷、二乙胺、哌嗪、乙二胺等为原料,合成了系列季戊四醇类单组分膨胀型阻燃剂。在合成季戊四醇磷酰氯中间体制备过程中,同时采用了普通合成方法和引入超声波技术合成方法,对比探讨了超声波对反应时间,温度的影响。在合成季戊四醇双磷酸酯二乙胺时,设计了正交实验,确定了最佳工艺条件.用红外与核磁对中间产物和最终产物进行结构表征,从而验证其结构组成是否与目标产物一致。通过热重分析(TG/DSC)对制得的三种阻燃剂的热稳定性进行测试,得出各种阻燃剂的初始分解温度及剩炭量,并通过高温马弗炉煅烧实验,确定膨胀型阻燃剂受热后膨胀成炭的能力,筛选出性能优良的膨胀型阻燃剂,并初步探讨磷、氮、碳三者协同作用对其膨胀成炭的能力的影响。同时,将其中两种制得的FIR与聚丙烯进行混炼,测定其氧指数(LOI)和拉伸强度,分析其力学性能。60119
关键词 膨胀型阻燃剂 季戊四醇 超声技术 热重分析
毕业设计说明书(毕业论文)外文摘要
Title Study on the synthesis of a novel pentaerythritol single-component series intumescent flame retardant
Abstract
In this paper, a series of pentaerythritol single-component intumescent flame retardant were synthesized which using pentaerythritol、phosphorus oxychloride、diethylamine、piperazine、ethidene diamine ,etc as raw matrial. The intermediate of these series IFR, pentaerythritol double phosphorus oxychloride, was synthesized under ordinary method and ultrasonic technique. Effects of ultrasonic on reaction time, reaction temperature were studied. The optimal reaction conditions of preparation of pentaerythritol double phosphate diethylamine were obtained through orthogonal experiment. According to the FTIR spectra and NMR spectra, the structures of intermediate final products were verified. Thermal stability of three kinds of IFR was tested through TG/DSC, their initial decomposition temperature were obtained as well as the amount of residual carbon. The ability of intumescing into carbon after heated of IFR was obtained through high temperature muffle furnace calcination experiment. The optimal IFR was selected and used to study the effect of synergy of phosphorus, nitrogen and carbon on the ability of intumescing into carbon. At the same time, respectively mixture two FIR made form synthetic experiments with polypropylene, determine their oxygen index and tensile strength to analysis their mechanical properties.
Keywords inrumescent flame retardants pentaerythritol ultrasonic technique TG/DSC
1 绪论 1
1. 1 阻燃剂的简介 1
1. 2 膨胀型阻燃剂(FIR) 1
1. 3 膨胀型阻燃剂的阻燃机理 3
1. 4 季戊四醇类膨胀型阻燃剂的应用 3
1. 5 本课题研究的主要内容及创新 4
2 新型季戊四醇类单质膨胀型阻燃剂的制备 6
2. 1 实验仪器及试剂 6
2. 2 实验原理及步骤