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嵌段共聚的聚酰胺6的合成与性能表征

发布时间:2019-01-02 10:36
【摘要】:热塑性弹性体在常温下具有橡胶弹性,在高温下可塑化,兼具塑料的流动性、可加工性和橡胶的弹性,广泛应用于医疗、电子配件、建筑、汽车行业、食品包装等众多领域。作为一种新型热塑性弹性体,聚酰胺系热塑性弹性体与聚氨酯和聚醚酯热塑性弹性体类似,都属于分段型嵌段聚合物,具有很好的应用前景。本文采用两步法(两个阶段)合成了具有分段型嵌段共聚物结构的聚酰胺6热塑性弹性体。第一阶段先合成具有双端羧基封端的预聚物聚酰胺6,第二阶段再与聚乙二醇(PEG)进行聚酯化反应生成聚酰胺6热塑性弹性体。研究了封端剂加入的时间、含量等对预聚物分子量的影响,优化了时间、温度、真空度、催化剂等合成工艺条件和参数。应用傅里叶红外光谱、氢谱核磁共振、热重分析仪、差示扫描量热仪、X射线衍射仪和扫描电镜表征了预聚物和聚酰胺6型热塑性弹性体的结构与性能。研究结果表明:1、预聚物的优化合成工艺为:240℃左右开环聚合4 h,加入封端剂1 h,抽真空1 h(真空度为0.05-0.07 MPa),嵌段共聚物合成的工艺条件:在温度为250℃反应下反应3 h,抽真空1 h(真空度0.05-0.07 MPa);2、傅里叶红外谱(FTIR)图中出现了醇类的亚甲基团的峰值,氢谱(1H-NMR)图中合成的产物具有聚酰胺6和聚乙二醇两者的峰值,表明嵌段共聚物合成成功;3、热重分析和差示扫描量热仪(DSC)测试说明共聚物在300℃以内具有良好的热稳定性,在-50~192℃的区间显示出良好的弹性性能,具有较宽的使用温度范围;4、XRD测试表明,软段的加入使一部分的α晶型转变成了γ晶型;5、SEM的测试表明软段使聚酰胺6热塑性弹性体具备橡胶弹性,但软硬段存在一定的不相容性。
[Abstract]:Thermoplastic elastomer has rubber elasticity at room temperature, plasticizing at high temperature, plastic fluidity, processability and rubber elasticity. It is widely used in many fields such as medical treatment, electronic accessories, construction, automobile industry, food packaging and so on. As a new thermoplastic elastomer, polyamide thermoplastic elastomer is similar to polyurethane and polyether ester thermoplastic elastomer. Polyamide 6 thermoplastic elastomer with segmented block copolymer structure was synthesized by two step method. In the first stage, the prepolymer polyamide 6 with double end carboxyl group was synthesized, and then the polyamide 6 thermoplastic elastomer was synthesized by polyesterification with polyethylene glycol (PEG) in the second stage. The effects of the time and content of the entrapment on the molecular weight of the prepolymer were studied, and the synthesis conditions and parameters such as time, temperature, vacuum degree, catalyst and so on were optimized. The structure and properties of the prepolymer and polyamide 6 thermoplastic elastomer were characterized by Fourier transform infrared spectroscopy, hydrogen NMR, thermogravimetric analyzer, differential scanning calorimetry, X-ray diffraction and scanning electron microscope. The results show that: 1. The optimum synthesis process of prepolymer is as follows: about 240 鈩,

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