【作者】 黄震；

【导师】 唐建国；

【作者基本信息】 青岛大学 ， 材料学， 2005， 硕士

【摘要】 本文采用S-B技术合成了两种芳香族酰胺化合物。对反应条件进行了探索和优化。着重考察了反应的温度、反应时间、反应的初始温度和升温速度、芳酰氯的滴加速度、溶剂用量、反应物的物料配比等因素对反应的影响,以寻求最佳的反应条件和合成工艺。将合成产物酰胺A和酰胺B用于聚合物的成核剂,并对其成核效果进行了测试。 本文以芳香族酰氯和脂肪族伯胺为原料,来制备芳香族酰胺化合物。产率可达到98%。实验结果表明,适当延长反应时间可提高产率。反应的初始温度愈高,升温速度愈快,产品的收率就愈高。增加任意一种反应物的量都可提高产率,但酰氯过量较胺过量来说,产品收率的增加更为明显。适当提高反应温度,可提高产率。本反应采取将一种反应物酰氯滴加到另一种反应物胺中的实验方法。酰氯的滴加速度愈慢,产品的收率就愈高。溶剂的使用量在不影响反应结果的情况下,应愈少愈好。可用DMSO作为重结晶溶剂对酰胺A进行重结晶。收率在76-78%。溶剂的循环使用不会影响产品的收率。但由于时间关系,对溶剂回收精制和循环使用的次数较少,实验数据还不够充分。 合成产物酰胺A和酰胺B可以用作饱和聚烯烃的成核剂。我们使用差示扫描量热法和偏光显微镜表征成核剂对饱和聚烯烃的成核效果。结果表明:该成核剂的加入均使结晶温度升高,结晶速度加快。并使结晶的尺寸细化,结晶规整均匀,从而使结晶度增大。更多还原

【Abstract】 In this paper, two triamines were prepared by a Schotten-Bauman reaction. The influence of reaction temperature, reaction time, ratio of reactants and the amount of the solvent were studied in order to find the optimal technological conditions. The procuct was purified by recrystallizition. Synthesize product the triamine A and triamine B can be used as nucleating agent of polyolefin and observe the nucleating effect of the nucleating agent.Trimines were prepared with aromatic acyl chloride and aliphatic amide by a Schotten-Bauman reaction. The product ratio can reach 98%. The result of experiments showed, Propriety extending of reaction time will improve the yield of the product. The beginning temperature of the reaction will lead to high yield. Increasing the amount of any of the two reactants will increase the product ratio. But more acyl chloride makes more product. Relevance increasing of reaction temperature will increase the product ratio. In this reaction, acyl chloride was dropped slowly into amine. The slower acyl chloride dropped, the higher the yield will be. The fewer consumption of the solvent, the higher the production ratio will become. DMSO was used as recrystal solvent to amide A and get a yield of 76-78%. The recycle times of the solvent will not affect the product ratio. As a result of not enough time, the reclaiming, refining and recycling times of the solvent are not enough, and the experiment data are not sufficiency.Synthesize product the triamine A and triamine B can be used as nucleating agent of polyolefin. Differential scanning calorimetry (DSC) and polarized optical microscopy were used to observe the nucleating effect of the nucleating agent. Compared with pure polyolefin, nucleated polyolefin showed a higher crystallization temperature and a faster crystallization rate. With the addition of nucleating agent, the spherulites became so small and even that the crystalline degree of nucleated polyolefin increased, which resulted in higher rigidity.更多还原