CAJ | 학술논문

采用液态聚碳硅烷与乙酰丙酮铝在常压下反应合成了具有不同铝含量的聚铝碳硅烷(PACS),由于不需要循环回流过程,因此该方法简单方便,安全性高.在与合成聚铝碳硅烷相同的条件下,对单纯的液态聚碳硅烷原料进行保温处理,所得产物的分析表征结果显示,该原料在反应条件下基本保持稳定,不会自聚或者裂解.不同铝含量的聚铝碳硅烷的元素分析结果表明,随着乙酰丙酮铝加入量的增加,聚铝碳硅烷中的铝含量增加,同时氧含量增加,氢含量减少,且乙酰丙酮铝中的铝元素几乎全部引入到液态聚碳硅烷中.GPC分析结果显示,随着铝含量的增大,PACS的数均分子量增大,分子量分布变宽.红外光谱和核磁共振波谱分析结果表明,液态聚碳硅烷与乙酰丙酮铝的反应主要以消耗Sj-H键的方式进行,铝元素以AlO_4,AlO_5和AlO_6 3种配位形式存在,同时形成Si-O-Al交联键,使得聚铝碳硅烷的分子量增大,分子量分布变宽.
채용액태취탄규완여을선병동려재상압하반응합성료구유불동려함량적취려탄규완(PACS),유우불수요순배회류과정,인차해방법간단방편,안전성고.재여합성취려탄규완상동적조건하,대단순적액태취탄규완원료진행보온처리,소득산물적분석표정결과현시,해원료재반응조건하기본보지은정,불회자취혹자렬해.불동려함량적취려탄규완적원소분석결과표명,수착을선병동려가입량적증가,취려탄규완중적려함량증가,동시양함량증가,경함량감소,차을선병동려중적려원소궤호전부인입도액태취탄규완중.GPC분석결과현시,수착려함량적증대,PACS적수균분자량증대,분자량분포변관.홍외광보화핵자공진파보분석결과표명,액태취탄규완여을선병동려적반응주요이소모Sj-H건적방식진행,려원소이AlO_4,AlO_5화AlO_6 3충배위형식존재,동시형성Si-O-Al교련건,사득취려탄규완적분자량증대,분자량분포변관.
Polyaluminocarbosilanes (PACS) with different Al contents were synthesized by reacting liquid polycarbosilane(LPCS) with aluminum acetylacetonate[Al(AcAc)_3]. Compared with those reported in literatures, this route is considered to be more convenient and safer since no circulating reflux is needed. It was shown that the composition and structure of LPCS heated and kept at the synthesis temperature of PACS remained fairly stable. The chemical elemental analysis results of PACS indicated that through this route the Al contents were almost fully introduced into PACS from Al (AcAc)_3, and with the increasing of Al contents, the O contents also increased. Furthermore, the formation of AlO_4, AlO_5 and AlO_6 was confirmed by ~(27)Al MAS NMR results. On the base of the structure analysis it was suggested that LPCS reacted with Al (AcAc)_3 by consuming Si-H bonds. Then Si-O-Al crosslinking bonds were formed, leading to the increases of the number average molecular weight and the polydispersion index in molecular weight with the increase of Al contents in PACS.