【作者】 郭岳；

【导师】 余自力；

【作者基本信息】 四川大学 ， 高分子化学与物理， 2005， 硕士

【摘要】 聚苯硫醚(PPS)是一种高性能的特种工程塑料,具有各种优异的性能。我国的PPS已经产业化,但反应的后处理技术落后,已经成为PPS产业发展的“瓶颈”。国内的PPS产品由于杂质含量高,不能满足电子电器以及一些具有特殊要求的用途。在电子封装材料方面,随着人民生活水品的逐渐提高,各国对环保的要求越来越高,因此用可回收的热塑性树脂对电子元器件进行封装是电子封装材料发展的重要方向。由于PPS在电磁屏蔽以及航天、军事领域的运用,美、日等公司对技术进行高度的垄断封锁,并且对我国不转让技术,不出售可用于尖端技术和军事目的的高性能PPS改性增强材料。因此,对PPS微粉制备、PPS纯化研究等提高PPS树脂档次的研究以及将PPS树脂用于封装材料研究具有重大的意义。 本文的内容有三个部分,第一部分综述了PPS的性能、用途、电子封装材料的组成、电子封装材料的现状、电子封装材料的发展方向、电子封装材料对填料以及PPS要求等。 第二部分是PPS微粉的制备研究和商品PPS的纯化研究。采用机械粉碎方法对商品PPS进行了粉碎,但PPS微粉的均匀性差,粉碎后的树脂需要经过分样筛按粒径分级后才能使用,并且由于树脂的静电作用,分级不能顺利进行,该法只能用于研究,不适合工业生产。研究发现,采用高温下能溶胀PPS的有机酰胺类溶剂或高温下能溶解PPS的高沸点芳香族化合物对PPS进行处理,可以得到PPS微粉,并且微粉粒径全部小于40μm,适合工业上大规模制造PPS微粉。采用PEG和NMP的混合溶剂对商品PPS进行了纯化处理研究,研究了PPS粒径、纯化温度、纯化时间、混合溶剂配比对纯化处理效果的影响,结果表明,树脂粒径越小、纯化温度越高,纯化效果越好。摸索的较好纯化处理条件为:树脂粒径通过80目筛,纯化温度200～220℃,纯化时间2～4小时,混合溶剂配比PEG:NMP为1:10。纯化后的PPS经检测表明,树脂中杂质离子含量和低聚物均显著降低,分别达到Na~+<30ppm、Li~+<3ppm、低聚物含量<0.5%,已达更多还原

【Abstract】 Poly(phenylene sulfide) (PPS) is a high-performance engineering plastics with many excellent properties. In China, although PPS has already been produced in industrialized scale, the post-treatment process of produced PPS is not developed yet. In a sense, the post-treatment process of PPS is become the "bottleneck" for PPS industrialization. Because the commercial PPS has many impurities in it, it can’t be used for some applications such as electronic encapsulation, fiber and film manufacture. In electronic encapsulation fields, the traditional thermosetting resin is gradually substituted by thermoplastic materials because the later is a recyclable materials, thus more and more countries developed many thermoplastic include PPS for electronic encapsulation. Because PPS can be used in the electromagnetic shielding, space flight and other military applications, the developed countries such as the United States, Japan forbid both the technique and the products to China strictly. Therefore, it is valuable to develop process for preparing PPS fine powder, high purity PPS and PPS based electronic encapsulation materials.This thesis consists of the following three parts. The first part introduces the properties and applications of PPS, the current situation of electronic encapsulation materials and their developing trends, PPS based electronic encapsulation materials, and the quality of PPS and fillers for producing electronic encapsulation materials.The second part concerns the preparation of the PPS fine powder and the purification process of PPS. Through mechanical grinding can produce PPS fine powder, the homogeneity of the obtained PPS fine powder is unsatisfactory, the resin after crushing needs to be sifted. So this method can only be used for studying, not suitable for industrial production. By treat with some organic amide and some otheraromatic solvents in high temperatures, we found that PPS can also be "crash" to fine powder with diameters less than 40uin. This process implies that it could be used for industrial production. The purification experiments shown that the mixture of PEG and NMP can eliminate the impurities contained in PPS effectively. The influence of PPS size, operating temperature, operating time and the ratio of two solvent have been investigated and the result shown that the best parameters for the purification of PPS are: PPS passing 80 mesh sieve, operating temperature 200-220 °C, operating time 2~4 hours, ratio of two solvents PEG/NMP=l/10. By treated under above-mentioned conditions, the purified PPS shows low impurity. The impurities contained in PPS is determined to be: Na’<30ppm , Li’<3ppm, oligomers<0.5%. These results are consistent with those for high purity PPS reported in literature, which suggest that the PPS by this treatment is suitable for electronic encapsulation. Repeat experiments show that this treatment has good reproducibility and is suitable for industrial production.The third part reported the research on the preparation of PPS based encapsulation materials. PPS .encapsulation materials are prepared by mixing purified PPS, fillers and other processing aids together by different ratio. The mixtures are extruded in two-screw extruder to strands and chopped to pellets, and then the pellets are injection molded to testing specimen for property measurements. The data of measurement shown that the thermal, mechanical, electrical properties and inflammability of obtained composite are similar to those of PPS electronic encapsulation materials reported by foreign company.更多还原