【作者】 杨勇；

【导师】 毋伟；

【作者基本信息】 北京化工大学 ， 化学工程与技术， 2013， 硕士

【摘要】 由于高分子材料燃烧时生成大量的浓烟及有毒气体,会严重危害公众的生命财产及生态环境,因此高分子材料的阻燃研究显得十分重要。在材料加工过程中加入阻燃剂是提高高分子材料阻燃性能的重要途径。三氧化二锑是一种常用的高效阻燃剂,但是因再生产过程中需消耗大量稀有的锑资源,其价格非常昂贵。以减少三氧化二锑的使用量为目的的复合技术及其应用研究就具有很大的意义。本文以硅灰石、氢氧化镁、高岭土为客体组分,制备了三氧化二锑复合颗粒,并研究了复合颗粒合成过程中的工艺条件及其应用性能。主要研究内容如下：1、以三氯化锑和针状硅灰石为原料,通过化学沉淀法制备了硅灰石-三氧化二锑(CaSiO3/Sb2O3)复合粒子,研究包覆量、反应温度、表面活性剂、硅灰石浆液浓度等工艺条件对包覆效果的影响,并对复合颗粒进行了表征和在聚酰胺6(PA6)体系中的阻燃性能和力学性能进行研究。研究表明,在优化的工艺条件下,三氧化二锑以超细粒子形式包覆在硅灰石表面,其中三氧化二锑晶型为斜方型、粒径约为80～120nm,并对制备工艺进行了放大实验。将放大实验得到的CaSiO3/Sb2O3复合粒子替代三氧化二锑加入到PA6树脂中,研究发现,将含有4.0份三氧化二锑的12份复合粒子代替6份三氧化二锑,可以达到工业上对PA6复合材料的阻燃要求,同时熔滴起始滴落的时间由3s延迟到9s；同时PA6复合材料的力学性能明显提高。2、以氢氧化镁、三氯化锑为原料,通过化学沉淀法制备了氢氧化镁-三氧化二锑(Mg(OH)2/Sb2O3)复合粒子,研究反应条件对复合颗粒包覆效果的影响,并对所得到的产物进行表征。在优化的工艺条件下,在六角片状氢氧化镁颗粒表面包覆一层晶型为斜方型、厚度为5～10nm、均匀的Sb2O3纳米膜。将含有4.2份三氧化二锑的15份Mg(OH)2/Sb2O3复合粒子替代6份三氧化二锑加入到PA6树脂中,可以达到工业上对PA6复合材料的阻燃要求,生烟量也有所减少,复合材料燃烧过程中没有熔滴产生；同时复合材料的力学性能显著提高。3、以高岭土、三氧化二锑为原料,通过机械力复合法,在精细研磨机中得到了高岭土-三氧化二锑(kaoline/Sb2O3)复合粒子,探讨了研磨时间及搅拌速度对复合颗粒的影响。将含有4.8份三氧化二锑的12份高岭土/Sb2O3复合粒子替代6份三氧化二锑加入到PA6树脂中,可以达到工业上对PA6复合材料的阻燃要求,复合材料燃烧过程中没有熔滴产生。同时复合材料的力学性能显著提高。更多还原

【Abstract】 Study of flame retardant is of great importance since polymer materials generate a lot of smoke and toxic gases when burned, which endangers public life and Eco-environment. The flame retardant agents are often added through the producing process of materials to improve the flame retardant property of polymer materials. Antimony trioxide is a commonly used efficient inorganic flame retardant, but it isvery expensive because it consumes too much of rare antimony resource through producing. It is of great point to do research for more efficient use of antimony trioxide through hybrid technology or its applications. In this paper, we prepared antimony trioxide composite particles using raw materials of wollastonite, Magnesium hydroxide and Kaoline. The synthesis conditions and its application were also discussed. The main points are listed below:1, The composite particles of CaSiO3/Sb2O3were prepared from the raw materials of wollastonite and antimony trichloride by chemical precipitation method. The effect of experimental conditions was discussed, such as coating amount, reaction temperature, surfactants and slurry concentration. The composite particles were characterized and the flame retardancy and mechanical properties of PA6composite materials were studied. The results show that the antimony trioxides were coated on the surface of wollastonite in the form of ultrafine particles under optimized process conditions. The composite particles of CaSiO3/Sb2O3were added to the PA6resin instead of antimony trioxide. The results showed that4parts of antimony trioxide in12parts of composite particles instead of6of parts antimony trioxide could meet the industry requirements for PA6composite materials. The time of droplet dripping was delayed from3s to9s and the mechanical properties of PA6composite materials were improved.2, The composite particles of Mg (OH)2/Sb2O3were prepared from the raw materials of Magnesium hydroxide and Antimony trichloride by chemical precipitation method. The effect of experimental conditions on the composite particles was discussed. The product obtained was characterized and the flame retardancy and mechanical properties of PA6composite materials were studied. The results showed that the surface of magnesium hydroxide particles with six-square sheet shape is coated on a layer thickness of5～10nm uniform Sb2O3nanometer film and the crystalline modifications of Sb2O3was orthorhombic polymorph. The results show that4.2parts of antimony trioxide in12parts of composite particles instead of6parts of antimony trioxide could meet the industry requirements for PA6composite materials. The flame retardancy experiment shows that the Mg (OH)2/Sb203had good flame retardant property in PA6composite materials and the amounts of smoke were also reduced. There were no phenomenon of droplet dripping and the mechanical properties of PA6composite materials were improved.3, The Kaoline/antimony trioxide (Kaoline/Sb2O3) composite particles were prepared by mechanic-chemical method using antimony trichloride and Kaoline. The effect of several parameters on the synthesized composites was investigated, such as stirring speed and grinding time. The results show that4.8parts of antimony trioxide in12parts of composite particles instead of6parts of antimony trioxide could meet the industry requirements for PA6composite materials. The flame retardancy experiment shows that the Kaoline/Sb2O3had good flame retardant property in PA6composite materials. There were no phenomenon of droplet dripping and the mechanical properties of PA6composite materials were improved.更多还原