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以镍为催化剂,定向聚合得到的顺—1,4—聚丁二烯(Ni—PB)具有较好的分子结构规整性。在适当的低温下,极易结晶。本文详细讨论了Ni—PB的溶胶及凝胶对低温结晶成核及生长的影响。采用燕山石化总公司,胜利化工厂生产的Ni—PB为样品。各样品的顺式含量均在92—96%之间。将0.5%Ni—PB甲苯溶液,在甘油表面上成膜、蒸馏水清洗后,捞在电镜载网上。经-30℃下不同时间结晶后,用OsO_4固定。在H—500型电镜下观察。 Ni—PB在-30℃下结晶的TEM照片给出可以得到尺寸为几+μm的球晶。其生长速率为1μm/min。对于凝胶含量较小的试样,结晶诱导期较长,晶核为单个片层或片层束(图a)。在片层的生长过程中,首先形成宽约为1000—2000A的界面不十分清晰的白色区,为预结晶区。进一步结晶,排列为规整的,有清晰界面的片层。如
Using nickel as catalyst, the cis-1,4-polybutadiene (Ni-PB) obtained by directional polymerization has good molecular structural regularity. In the appropriate low temperature, easily crystallized. In this paper, the effects of Ni-PB sol and gel on the nucleation and growth of low-temperature crystallization were discussed in detail. Using Yanshan Petrochemical Corporation, Shengli Chemical Factory production of Ni-PB samples. The cis content of each sample was between 92-96%. 0.5% Ni-PB toluene solution, a film on the surface of glycerol, distilled water, after cleaning, fishing in the electron microscope network. After crystallization at -30 ℃ for different time, fixed with OsO_4. Observed under H-500 electron microscope. A TEM photograph of Ni-PB crystallized at -30 ° C gives spherulites in the size of a few + μm. Its growth rate is 1μm / min. For the samples with smaller gel content, the crystallization induction period is longer and the nuclei are single slices or sheet bundles (Fig. A). In the growth of the lamella, the first to form a wide area of about 1000-2000A interface is not very clear white area, pre-crystallization zone. Further crystallization, arranged as a regular, clear layer of the interface. Such as