微胶囊包覆聚磷酸铵的制备及膨胀型阻燃剂对PP阻燃性能的研究

发布时间：2018-03-31 13:52

本文选题：密胺树脂　切入点：微胶囊包覆　出处：《华东理工大学》2017年硕士论文

【摘要】：随着人们安全和环保意识的提高,膨胀型阻燃剂(IFR)作为一种无卤、高效的阻燃剂在聚合物阻燃中得到广泛的应用。但是,作为膨胀型阻燃剂体系重要组成部分,聚磷酸铵(APP)存在耐水性差、易团聚和与基材相容性差等缺点,严重影响了膨胀型阻燃剂的使用效果。本文通过微胶囊包覆改性APP,提高其耐水性、与基材相容性,进一步究了 IFR对聚丙烯(PP)阻燃效果。首先,用密胺树脂对APP进行微胶囊包覆改性,制备包覆产物MFAPP。实验研究了温度、时间、pH、壳芯比、水/乙醇溶剂比等因素对密胺树脂包覆APP效果的影响,并通过溶解度、分散性、粘度等表征确立了最佳包覆工艺。对APP、MFAPP进行红外、SEM、TG、阻燃性能、耐水性的表征,结果表明,密胺树脂成功实现了对APP的包覆,且MFAPP包覆效果良好,不仅提高了 APP耐水性及与PP的相容性,阻燃性也得到提高。当分别添加30%APP、MFAPP到PP中时,APP/PP复合材料氧指数为21.5%,未达到任何阻燃级别;而MFAPP/PP复合材料氧指数为29.5%,且达到V-1阻燃级别,经过耐水性处理仍达到29.0%。其次,为了进一步提高包覆产物的热稳定性和阻燃性能,实验采用原位聚合的方法,首先用正硅酸乙酯改性密胺树脂,然后将其作为壳材对APP进行包覆,制备了具有核壳结构的SIMFAPP。实验研究了温度、时间、pH、壳芯比等因素对正硅酸乙酯改性密胺树脂包覆APP的影响,通过溶解度、表面元素分析(EDS)的表征确立了包覆最佳工艺。并通过红外、SEM、TG、氧指数、UL-94和耐水性等手段进行表征,结果表明,正硅酸乙酯成功改性密胺树脂,且完成了对APP包覆;SIMFAPP仍具有较强的耐水性和相容性,表面含有大量Si元素,热稳定性得到明显提高;当分别添加30%SIMFAPP到PP中时,MFAPP/PP复合材料氧指数为32.5%,达到V-0级,经过耐水性处理仍达到31.6%。最后,考察了 IFR对PP阻燃性能影响。在IFR总量为30%的情况下,分别将APP/PER、MFAPP/PER、SIMFAPP/PER按不同的比例添加到PP,研究了 APP包覆前后与PER协同阻燃对PP阻燃性能影响,并通过LOI、UL-94、TG、SEM等对复合材料阻燃性能、热稳定性和残炭表面结构进行了分析。实验结果表明,APP/PER、MFAPP/PER、SIMFAPP/PER协同阻燃起到很好的阻燃效果,随着APP、MFAPP、SIMFAPP比例增加阻燃性增强,热稳定性提高;且PP/SIMFAPP/PER复合材料阻燃性和热稳定性明显高于PP/MFAPP/PER、PP/APP/PER 复合材料。
[Abstract]:With the increasing awareness of safety and environmental protection, the intumescent flame retardant (IFR) has been widely used as a halogen-free and highly effective flame retardant in polymer flame retardants, but as an important component of the intumescent flame retardant system. The poor water resistance, easy agglomeration and poor compatibility with the substrate have seriously affected the application effect of the intumescent flame retardant. In this paper, the water resistance and compatibility with the substrate were improved by coating the APP with microcapsules. The flame retardant effect of IFR on PP was further investigated. Firstly, the microencapsulated APP was modified with melamine resin to prepare the coating product MFAPP. The temperature, time, pH and the ratio of shell to core were studied experimentally. The effect of water / ethanol solvent ratio on the coating effect of melamine resin on APP was studied. The optimum coating process was established by the characterization of solubility, dispersion and viscosity. The melamine resin was successfully coated with APP, and the coating effect of MFAPP was good, which not only improved the water resistance of APP and its compatibility with PP. The flame retardancy was also improved. When 30 APP MFAPP was added to PP, the oxygen index of PP / PP composites was 21.5, which did not reach any flame-retardant level, while the oxygen index of MFAPP/PP composites was 29.5and reached the V-1 flame-retardant grade. In order to further improve the thermal stability and flame retardancy of the coating products, in situ polymerization was used to modify the melamine resin with ethyl orthosilicate, and then APP was coated as the shell material. SIMFAPP with core-shell structure was prepared. The effects of temperature, time, pH and ratio of shell to core on APP coated with melamine resin modified by ethyl orthosilicate were studied. The optimum coating process was established by means of surface element analysis (EDS), and characterized by IR, TG, UL-94 and water resistance. The results showed that the melamine resin was modified successfully by ethyl orthosilicate. The APP coated SIMFAPP still has strong water resistance and compatibility, there are a lot of Si elements on the surface, the thermal stability is improved obviously, and the oxygen index of MFAPP / PP composites is 32.5 and reaches V-0 when 30%SIMFAPP is added to PP separately. Finally, the effect of IFR on the flame retardancy of PP was investigated. Under the condition of 30% IFR, the effects of synergistic flame retardancy of APP and PER on the flame retardancy of PP were studied by adding app / P / P SIMFAPP / per in different proportions, respectively. The flame retardancy, thermal stability and surface structure of carbon residue were analyzed by loi UL-94 TGG SEM. The experimental results showed that the synergistic flame retardant effect of app / per / per / MFAPP / SIMFAPP / per increased with the increase of APP / MFAPP / SIMFAPP ratio, and the thermal stability of the composites was improved with the increase of APP / MFAPP / SIMFAPP ratio. The flame retardancy and thermal stability of PP/SIMFAPP/PER composites were significantly higher than those of PP / MFAP / P / PP / PP / per composites.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ325.14

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