高耐热聚芳醚酮固化邻苯二甲腈树脂
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1.精细化工国家重点实验室 大连理工大学 化工学院 高分子材料系, 山西新华防化装备研究院有限公司;2.精细化工国家重点实验室 大连理工大学 化工学院 高分子材料系

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TQ630

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国家自然科学基金(基金号 51673033,51873027);中央高校基本科研业务费(项目号 DUT20TD114)资助项目


Curing of Phthalonitrile Resin with High-temperature Resistant Poly (phthalazinone ether ketone)
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1.State Key Laboratory of Fine Chemical, Department of Polymer Science &2.Materials, School of Chemical Engineering, Dalian University of Technology;3.2. Shanxi Xinhua Chemical Defense Equipment Research Inst

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    摘要:

    以4-(4-羟基苯基)-2,3-二氮杂萘-1-酮、4,4’-二氟二苯甲酮和4-氨基苯酚为原料,通过两步一锅法合成了一种新型的氨基封端杂萘联苯聚芳醚酮(A-PPEK),并考察了其对邻苯二甲腈树脂的固化性能。相比于常用的芳香二胺固化剂4,4’-二氨基二苯砜(DDS),A-PPEK的5%热失重温度提高了69.3 ℃。另外,与DDS在400 ℃时快速升华不同,A-PPEK在相同温度下仍能保留95%以上的质量,说明A-PPEK可以有效解决小分子固化剂高温下分解在邻苯二甲腈树脂中造成缺陷的问题。一系列试验表明,以A-PPEK固化间苯二酚邻苯二甲腈树脂DPPH,体系具有优异的耐热性和加工流动性:固化树脂的5%热失重温度最高可达553.2 ℃,玻璃化转变温度高于实验测试温度380 ℃,最低粘度可至0.2 Pa?S。

    Abstract:

    A novel amino terminated poly(phthalazinone ether ketone) (A-PPEK) was synthesized from 4-(4-hydroxylphenyl)(2H)-phthalazin-1-one, 4,4'-difluoro benzophenone and 4-aminophenol by a two-step one pot method, and its curing properties for phthalonitrile resin were investigated. Compared with the commonly used aromatic diamine curing agent 4,4 '-diaminodiphenyl sulfone (DDS), the 5% weight loss temperature of A-PPEK was increased by 69.3 ℃. Moreover, unlike the rapid sublimation of DDS at 400 ℃, A-PPEK can still retain more than 95% of the mass at the same temperature, indicating that A-PPEK can effectively solve the problem of defects in phthalonitrile resin caused by the decomposition of small molecule curing agent at high temperature. A series of tests showed that the system of resorcinol phthalonitrile resin DPPH cured with A-PPEK had excellent heat resistance and processability: the maximum 5% weight loss temperature of the cured resin can reach 553.2 ℃, the glass transition temperature was higher than the experimental test temperature of 380 ℃, and the minimum viscosity can reach 0.2 Pa?s.

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胡月,马守骏,蹇锡高,翁志焕.高耐热聚芳醚酮固化邻苯二甲腈树脂[J].精细化工,2023,40(4):

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  • 收稿日期:2022-07-19
  • 最后修改日期:2022-09-25
  • 录用日期:2022-10-06
  • 在线发布日期: 2023-06-12
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