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微膠囊包覆聚磷酸銨的制備及膨脹型阻燃劑對PP阻燃性能的研究

發(fā)布時間:2018-03-31 13:52

  本文選題:密胺樹脂 切入點:微膠囊包覆 出處:《華東理工大學(xué)》2017年碩士論文


【摘要】:隨著人們安全和環(huán)保意識的提高,膨脹型阻燃劑(IFR)作為一種無鹵、高效的阻燃劑在聚合物阻燃中得到廣泛的應(yīng)用。但是,作為膨脹型阻燃劑體系重要組成部分,聚磷酸銨(APP)存在耐水性差、易團聚和與基材相容性差等缺點,嚴重影響了膨脹型阻燃劑的使用效果。本文通過微膠囊包覆改性APP,提高其耐水性、與基材相容性,進一步究了 IFR對聚丙烯(PP)阻燃效果。首先,用密胺樹脂對APP進行微膠囊包覆改性,制備包覆產(chǎn)物MFAPP。實驗研究了溫度、時間、pH、殼芯比、水/乙醇溶劑比等因素對密胺樹脂包覆APP效果的影響,并通過溶解度、分散性、粘度等表征確立了最佳包覆工藝。對APP、MFAPP進行紅外、SEM、TG、阻燃性能、耐水性的表征,結(jié)果表明,密胺樹脂成功實現(xiàn)了對APP的包覆,且MFAPP包覆效果良好,不僅提高了 APP耐水性及與PP的相容性,阻燃性也得到提高。當分別添加30%APP、MFAPP到PP中時,APP/PP復(fù)合材料氧指數(shù)為21.5%,未達到任何阻燃級別;而MFAPP/PP復(fù)合材料氧指數(shù)為29.5%,且達到V-1阻燃級別,經(jīng)過耐水性處理仍達到29.0%。其次,為了進一步提高包覆產(chǎn)物的熱穩(wěn)定性和阻燃性能,實驗采用原位聚合的方法,首先用正硅酸乙酯改性密胺樹脂,然后將其作為殼材對APP進行包覆,制備了具有核殼結(jié)構(gòu)的SIMFAPP。實驗研究了溫度、時間、pH、殼芯比等因素對正硅酸乙酯改性密胺樹脂包覆APP的影響,通過溶解度、表面元素分析(EDS)的表征確立了包覆最佳工藝。并通過紅外、SEM、TG、氧指數(shù)、UL-94和耐水性等手段進行表征,結(jié)果表明,正硅酸乙酯成功改性密胺樹脂,且完成了對APP包覆;SIMFAPP仍具有較強的耐水性和相容性,表面含有大量Si元素,熱穩(wěn)定性得到明顯提高;當分別添加30%SIMFAPP到PP中時,MFAPP/PP復(fù)合材料氧指數(shù)為32.5%,達到V-0級,經(jīng)過耐水性處理仍達到31.6%。最后,考察了 IFR對PP阻燃性能影響。在IFR總量為30%的情況下,分別將APP/PER、MFAPP/PER、SIMFAPP/PER按不同的比例添加到PP,研究了 APP包覆前后與PER協(xié)同阻燃對PP阻燃性能影響,并通過LOI、UL-94、TG、SEM等對復(fù)合材料阻燃性能、熱穩(wěn)定性和殘?zhí)勘砻娼Y(jié)構(gòu)進行了分析。實驗結(jié)果表明,APP/PER、MFAPP/PER、SIMFAPP/PER協(xié)同阻燃起到很好的阻燃效果,隨著APP、MFAPP、SIMFAPP比例增加阻燃性增強,熱穩(wěn)定性提高;且PP/SIMFAPP/PER復(fù)合材料阻燃性和熱穩(wěn)定性明顯高于PP/MFAPP/PER、PP/APP/PER 復(fù)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.
【學(xué)位授予單位】:華東理工大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:TQ325.14

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