含醚砜芳香二胺单体的合成及热塑性聚酰亚胺的制备研究

Synthesis of Aromatic Diamine Monomer with Ether and Sulfone Groups and Properties of Thermoplastic Polyimide

在碳酸钾的催化作用下,采用对氨基苯酚和4,4′-二氯二苯砜反应得到双[4-(4-氨基苯氧基)苯基]砜(BAPS)。通过熔点测试、高效液相色谱测试、FT-IR和1H-NMR分析,验证了产物BAPS的结构,其纯度为99.21%,满足作为芳香二胺单体用来合成聚酰亚胺的要求。然后将芳香二胺BAPS、ODA与芳香二酐ODPA通过共聚反应合成了较高黏度和分子量的聚酰胺酸溶液,并制备了热塑性聚酰亚胺薄膜。通过熔体流动速率、DSC、TGA等测试发现,热塑性聚酰亚胺薄膜具有一定的热塑性(初始熔融温度约310℃)、较高的玻璃化转变温度(249℃)和较好的热稳定性(热失重10%的温度约为510℃,800℃残炭率约为18%)。

A bis[4-（4-aminophenoxy）phenyl]sulfone （BAPS） was synthesized from p-aminophenol and 4,4′-dichloro diphenyl sulfone under the catalysis of potassium carbonate, and its structure was verified by melting point, HPLC, FT-IR and ^1H-NMR test. Its purity is 99.21%, which satisfy the requirements of aromatic diamine monomer for synthesis of polyimide. Then a polyamide acid solution with higher viscos-ity and molecular weight was synthesized from aromatic diamine BAPS, ODA and aromatic dianhydride ODPA, and the thermoplastic polyimide film was prepared. The melt flow rate, DSC, and TGA test results show that the thermoplastic polyimide film has good thermoplastic （the initial melting temperature is about 310 ℃）, high Tg （249 ℃）, and excellent thermal stability （the 10% weight loss temperature is about 510℃, the char yield at 800℃ is about 18%）.