绝缘材料
絕緣材料
절연재료
Insulating Materials
2015年
11期
22-25,30
,共5页
严辉%李桢林%张雪平%杨志兰%范和平
嚴輝%李楨林%張雪平%楊誌蘭%範和平
엄휘%리정림%장설평%양지란%범화평
含醚砜芳香二胺%热塑性聚酰亚胺%合成
含醚砜芳香二胺%熱塑性聚酰亞胺%閤成
함미풍방향이알%열소성취선아알%합성
aromatic diamine monomer with ether and sulfone groups%thermoplastic polyimide%synthesis
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%)。
在碳痠鉀的催化作用下,採用對氨基苯酚和4,4′-二氯二苯砜反應得到雙[4-(4-氨基苯氧基)苯基]砜(BAPS)。通過鎔點測試、高效液相色譜測試、FT-IR和1H-NMR分析,驗證瞭產物BAPS的結構,其純度為99.21%,滿足作為芳香二胺單體用來閤成聚酰亞胺的要求。然後將芳香二胺BAPS、ODA與芳香二酐ODPA通過共聚反應閤成瞭較高黏度和分子量的聚酰胺痠溶液,併製備瞭熱塑性聚酰亞胺薄膜。通過鎔體流動速率、DSC、TGA等測試髮現,熱塑性聚酰亞胺薄膜具有一定的熱塑性(初始鎔融溫度約310℃)、較高的玻璃化轉變溫度(249℃)和較好的熱穩定性(熱失重10%的溫度約為510℃,800℃殘炭率約為18%)。
재탄산갑적최화작용하,채용대안기분분화4,4′-이록이분풍반응득도쌍[4-(4-안기분양기)분기]풍(BAPS)。통과용점측시、고효액상색보측시、FT-IR화1H-NMR분석,험증료산물BAPS적결구,기순도위99.21%,만족작위방향이알단체용래합성취선아알적요구。연후장방향이알BAPS、ODA여방향이항ODPA통과공취반응합성료교고점도화분자량적취선알산용액,병제비료열소성취선아알박막。통과용체류동속솔、DSC、TGA등측시발현,열소성취선아알박막구유일정적열소성(초시용융온도약310℃)、교고적파리화전변온도(249℃)화교호적열은정성(열실중10%적온도약위510℃,800℃잔탄솔약위18%)。
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%).